Triethylamine → 5-(N-(3-((N-(Biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxyphenylsulfonamido)methyl)benzyl)sulfamoyl)-2-methylbenzoic acid

HRID 1889653

反応式

[NH2:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:33]=[CH:34][CH:35]=1)[CH2:6][N:7]([CH2:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[CH:23][CH:22]=1)[S:8]([C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[C:12]=1[OH:19])(=[O:10])=[O:9].CCN(CC)CC.Cl[S:44]([C:47]1[CH:48]=[CH:49][C:50]([CH3:56])=[C:51]([CH:55]=1)[C:52]([OH:54])=[O:53])(=[O:46])=[O:45]>C(Cl)Cl>[C:24]1([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[CH:25]=[CH:26][C:21]([CH2:20][N:7]([CH2:6][C:5]2[CH:4]=[C:3]([CH:35]=[CH:34][CH:33]=2)[CH2:2][NH:1][S:44]([C:47]2[CH:48]=[CH:49][C:50]([CH3:56])=[C:51]([CH:55]=2)[C:52]([OH:54])=[O:53])(=[O:46])=[O:45])[S:8]([C:11]2[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[C:12]=2[OH:19])(=[O:10])=[O:9])=[CH:22][CH:23]=1

参加物

実験手順

To a solution of N-(3-(aminomethyl)benzyl)-N-(biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxybenzenesulfonamide (50 mg, 0.095 mmol) and Et3N (0.13 mL) in CH2Cl2 (4 mL) was added a solid of 5-(chlorosulfonyl)-2-methylbenzoic acid (22.24 mg, 0.095 mmol) at rt and it was stirred at it for 70 min. Direct purification of the mixture after concentration by prep HPLC provided the desired product (40 mg, 58.1%) as a white solid after lyophilization. 1H NMR (CD3OD): δ 8.17 (d, J=2.0 Hz, 1H), 7.93 (dd, J=8.3, 2.2 Hz, 1H), 7.56˜6.90 (m, 15H), 6.76 (s, 1H), 4.34 (s, 2H), 4.31 (s, 2H), 3.87 (s, 2H), 2.52 (s, 3H); MS (ESI): (M+H)+=725.

後処理

customDirect purification of the mixture
concentrationafter concentration by prep HPLC

出典と根拠

ORDレコード: ord-70127a297d67473496f5e005ad3600ef
出典データセット: uspto-grants-2013_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08501992B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

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