Sodium Hydroxide → HCID 11670217、化合物

HRID 855988ノート

反応式

HRID 855988 の反応式
[OH-].[Na+].C[O:4][C:5](=[O:35])[C:6]1[CH:11]=[C:10]([S:12](=[O:33])(=[O:32])[NH:13][C:14]2[CH:19]=[CH:18][C:17]([S:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=3)=[CH:16][CH:15]=2)[CH:9]=[CH:8][C:7]=1[CH3:34]>CO>[CH3:34][C:7]1[CH:8]=[CH:9][C:10]([S:12](=[O:33])(=[O:32])[NH:13][C:14]2[CH:15]=[CH:16][C:17]([S:20][CH2:21][C:22]3[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=3)=[CH:18][CH:19]=2)=[CH:11][C:6]=1[C:5]([OH:35])=[O:4]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 58937034HCID 58937034、化合物

生成物 1

HCID 11670217HCID 11670217、化合物収率 94%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1.0N aqueous sodium hydroxide (9.1 ml, 9.16 mmol) was added to a solution of 2-methyl-5-[4-(4-trifluoromethyl-benzylsulfanyl)-phenylsulfamoyl]-benzoic acid methyl ester (1.13 g, 2.29 mmol) in 100 ml methanol and the resulting solution was heated at reflux overnight under nitrogen. The reaction solution was then cooled to room temperature and concentrated under reduced pressure. The residue was stirred in 1.0N aqueous hydrochloric acid solution (25 ml) and filtered to yield the title compound as a white solid (1.03 g, 94% yield). MS: 480.2 (M−1); 1H NMR (400 MHz, CD3OD): δ2.49 (s, 3H), 4.04 (s, 2H), 6.96 (d, 2H), 7.1 (d, 2H), 7.29 (m, 2H), 7.33 (d, 1H), 7.47 (m, 3H), 7.94 (b, 1H).

後処理

  1. temperaturethe resulting solution was heated
  2. temperatureat reflux overnight under nitrogen
  3. concentrationconcentrated under reduced pressure
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-82bd0a81e6d2451e88ddb4f8ca1607bb
出典データセット
uspto-grants-2007_08
特許番号
US07262318B2

反応ノート

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