Sodium Hydroxide → HCID 11670217, 화합물

HRID 855988노트

반응식

HRID 855988 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 58937034HCID 58937034, 화합물

생성물 1

HCID 11670217HCID 11670217, 화합물수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-82bd0a81e6d2451e88ddb4f8ca1607bb
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262318B2

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