1-(6-Bromonaphthalene-2-sulfonyl)piperazine → HCID 178432520、化合物

HRID 1937320ノート

反応式

HRID 1937320 の反応式
Cl.[CH3:2][C:3]1[NH:4][CH:5]=[C:6]([C:8]2[CH:16]=[CH:15][C:11]([C:12]([OH:14])=O)=[CH:10][CH:9]=2)[N:7]=1.[Br:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][CH:27]=1)[CH:24]=[C:23]([S:28]([N:31]1[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]1)(=[O:30])=[O:29])[CH:22]=[CH:21]2>C(O)C.CCCCCC>[Br:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][CH:27]=1)[CH:24]=[C:23]([S:28]([N:31]1[CH2:32][CH2:33][N:34]([C:12](=[O:14])[C:11]3[CH:10]=[CH:9][C:8]([C:6]4[N:7]=[C:3]([CH3:2])[NH:4][CH:5]=4)=[CH:16][CH:15]=3)[CH2:35][CH2:36]1)(=[O:29])=[O:30])[CH:22]=[CH:21]2

参加物

4

反応物 2

HCID 223297091-(6-Bromonaphthalene-2-sulfonyl)piperazineHCID 178432525HCID 178432525、化合物

生成物 1

HCID 178432520HCID 178432520、化合物収率 85%

試薬・触媒・溶媒 1

HCID 21879635Ethanol hexane溶媒

実験手順

By an exactly analogous method to that described in Example 1, starting from 4-(2-methylimidazol-4-yl)benzoic acid hydrochloride and 1-(6-bromonaphth-2-ylsulphonyl)piperazine was prepared 1-(6-bromonaphth-2-ylsulphonyl)-4-[4-(2-methylimidazol-4-yl)benzoyl]piperazine (423 mg, 85% yield), m.p. 215-216° C. (from ethanol/hexane), 1H NMR (d6DMSO) 2.3 ppm (s,3H), 3.0-3.2 ppm (broad s,4H), 3.4-3.7 ppm (broad s,4H), 7.2 ppm (d,2H), 7.5 ppm (s,1H), 7.7 ppm (d,2H), 7.8 ppm (t,2H), 8.2 ppm (t,2H), 8.4 ppm (s,1H), 8.45 ppm (s,1H), 11.8 ppm (broad s,1H), the spectrum also contained signals due to ethanol (˜0.33 mol eq.); microanalysis, found: C, 55.4; H, 4.8; N, 9.9; S, 5.8%; C25H23N4O3BrS requires: C, 55.6; H, 4.5; N, 10.1; S, 5.8%; MS (M+H)+ 539/541.

出典と根拠

ORDレコード
ord-b047de670fc247f79074198c80ac3564
出典データセット
uspto-grants-2002_05
特許番号
US06395731B1

反応ノート

読み込み中…