1-(6-Bromonaphthalene-2-sulfonyl)piperazine → 1-(6-Bromonaphth-2-ylsulphonyl)-4-[4-(1-imidazolyl)benzoyl]piperazine

HRID 1937319노트

반응식

HRID 1937319 반응식
Cl.[N:2]1([C:7]2[CH:15]=[CH:14][C:10]([C:11]([OH:13])=O)=[CH:9][CH:8]=2)[CH:6]=[CH:5][N:4]=[CH:3]1.[Br:16][C:17]1[CH:18]=[C:19]2[C:24](=[CH:25][CH:26]=1)[CH:23]=[C:22]([S:27]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)(=[O:29])=[O:28])[CH:21]=[CH:20]2>C(O)C.CCCCCC>[Br:16][C:17]1[CH:18]=[C:19]2[C:24](=[CH:25][CH:26]=1)[CH:23]=[C:22]([S:27]([N:30]1[CH2:31][CH2:32][N:33]([C:11](=[O:13])[C:10]3[CH:9]=[CH:8][C:7]([N:2]4[CH:6]=[CH:5][N:4]=[CH:3]4)=[CH:15][CH:14]=3)[CH2:34][CH2:35]1)(=[O:28])=[O:29])[CH:21]=[CH:20]2

참가 물질

4

반응물 2

HCID 223297091-(6-Bromonaphthalene-2-sulfonyl)piperazineHCID 43810723HCID 43810723, 화합물

생성물 1

HCID 99366531-(6-Bromonaphth-2-ylsulphonyl)-4-[4-(1-imidazolyl)benzoyl]piperazine수율 85%

시약·촉매·용매 1

HCID 21879635Ethanol hexane용매

실험 절차

By an exactly analogous method to that described in Example 1, starting from 4-(1-imidazolyl)benzoic acid hydrochloride and 1-(6-bromonaphth-2-ylsulphonyl)piperazine was prepared 1-(6-bromonaphth-2-ylsulphonyl)-4-[4-(1-imidazolyl)benzoyl]piperazine (444 mg, 85% yield), m.p. 207-209° C. (from ethanol/hexane), 1H NMR (d6DMSO) 3.0-3.2 ppm (broad s,4H), 3.5-3.8 ppm (broad s,4H), 7.1 ppm (s,1H), 7.4 ppm (d,2H), 7.6 ppm (d,2H), 7.75 ppm (s,1H), 7.8 ppm (t,2H), 8.2 ppm (t,2H), 8.3 ppm (s,1H), 8.4 ppm (s,1H), 8.45 ppm (s,1H), the spectrum also contained signals due to ethanol (<0.2 mol eq.); microanalysis, found: C, 55.0; H, 4.3; N, 10.4; S, 6.2%; C24H21N4O3BrS requires: C, 54.9; H, 4.0; N, 10.7; S, 6.1%; MS (M+H)+ 525/527.

출처 및 근거

ORD 기록
ord-825fbdc12d5446ffbbea31d48c250cdc
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06395731B1

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