PIPERAZIN HYDRAT

Piperazini hydras

 

C4H10N2.6H2O P.t.l: 194,2

Piperazin hydrat phai cha t 98,0 en 101,0% C4H10N2. 6H2O.

Tnh chat

Tinh the khong mau, de chay nc.

De tan trong nc va ethanol 96%, rat kho tan trong ether.

Chay khoang 43 oC.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A.

Nhom II: B, C.

A. Pho hong ngoai (Phu luc 4.2) cua che pham phai phu hp vi pho hong ngoai cua piperazin hydrat chuan (C). Lam kho che pham va chat chuan tren phosphor pentoxyd (TT), trong chan khong, trong 48 gi. Nghien thanh bot, tranh hut nc, ep a va ghi pho ngay.

B. Trong muc th Tap chat lien quan, quan sat ban mong sau khi phun cac dung dch ninhydrin: vet chnh thu c t dung dch th (2) phai tng t ve v tr, mau sac va kch thc so vi vet chnh thu c t dung dch oi chieu (1).

C. Hoa tan 0,5 g che pham trong 5 ml dung dch natri hydroxyd loang (TT), them 0,2 ml benzoyl clorid (TT) tron eu. Tiep tuc them tng phan 0,2 ml benzoyl clorid (TT) en khi khong con tua tao thanh. Loc va ra tua nhieu lan vi tong cong 10 ml nc. Hoa tan tua trong 2 ml ethanol 96% (TT) nong, cho dung dch nay vao 5 ml nc. e yen 4 gi, loc, ra tinh the bang nc va say kho t 100 en 105 oC. Tinh the chay t 191 en 196 oC (Phu luc 6.7).

o trong va mau sac cua dung dch

Dung dch S: Hoa tan 1,0 g che pham trong nc khong co carbon dioxyd (TT) va pha loang thanh 20 ml bang cung dung moi.

Dung dch S phai trong (Phu luc 9.2) va co mau khong c tham hn mau mau N8 (Phu luc 9.3, phng phap 2).

pH

Dung dch S co pH t 10,5 en 12,0 (Phu luc 6.2).

Tap chat lien quan

Xac nh bang phng phap sac ky lp mong (Phu luc 5.4).

Ban mong: Silica gel G (TT).

Dung moi khai trien: Amoniac am ac - aceton (20 : 80) va mi pha.

Dung moi hoa tan: Hn hp ethanol - amoniac am ac (2 : 3)

Dung dch th (1): Hoa tan 1,0 g che pham trong 6 ml dung dch amoniac am ac va pha loang thanh 10 ml bng ethanol (TT).

Dung dch th (2): Pha loang 1 ml dung dch th (1) bang dung moi hoa tan va pha loang thanh 10 ml vi cung dung moi.

Dung dch oi chieu (1): Hoa tan 0,1 g piperazin hydrat chuan (TT) trong dung moi hoa tan va pha loang thanh 10 ml vi cung dung moi.

Dung dch oi chieu (2): Hoa tan 25 mg ethylendiamin (TT) trong dung moi hoa tan va pha loang thanh 100 ml vi cung dung moi.

Dung dch oi chieu (3): Hoa tan 25 mg triethylendiamin (TT) trong dung moi hoa tan va pha loang thanh 100 ml vi cung dung moi.

Dung dch oi chieu (4): Hoa tan 12,5 mg triethylendiamin (TT) trong 5,0 ml dung dch th (1) va pha loang thanh 50 ml vi cung dung moi.

Cach tien hanh: Cham rieng biet len ban mong 5 ml moi dung dch tren. Trien khai sac ky en khi dung moi i c 15 cm. Say ban mong 105 oC va phun lan lt dung dch ninhydrin 0,3% trong hon hp gom acid acetic khan (TT) va butanol (TT) (3 : 100), dung dch ninhydrin 0,15% trong ethanol (TT). Say ban mong 105 oC trong 10 phut.

Tren sac ky o bat ky vet phu nao thu c t dung dch th (1) khong c am mau hn vet thu c t dung dch oi chieu (2) (0,25%).

Phun len ban mong dung dch iod 0,1 N va e khoang 10 phut. Vet tng ng vi triethylendiamin (TT) thu c t dung dch th (1) khong c am mau hn vet thu c t dung dch oi chieu (3). Phep th ch co gia tr khi dung dch oi chieu (4) cho 2 vet tach ro rang.

Kim loai nang

Khong c qua 20 phan trieu (Phu luc 9.4.8).

Lay 12 ml dung dch S tien hanh th theo phng phap 1. Dung dung dch ch mau 1 phan trieu (TT) e chuan b mau oi chieu.

Tro sulfat

Khong c qua 0,1% (Phu luc 9.9, phng phap 2).

Dung 1,0 g che pham.

nh lng

Hoa tan 80,0 mg che pham trong 10 ml acid acetic khan (TT) bang cach un nong nhe va pha loang thanh 70 ml vi cung dung moi. Chuan o bang dung dch acid percloric 0,1 N (C), dung 0,25 ml dung dch 1-naphtholbenzein (TT) lam ch th, en khi mau chuyen t vang nau sang xanh luc.

1 ml dung dch acid percloric 0,1 N (C) tng ng vi 9,705 mg C4H10N2. 6H2O.

Bao quan

Trong lo kn va tranh anh sang.

Loai thuoc

Tr giun san.