Water → 4-Chloro-2-methyl-5-phenylisothiazol-3(2H)-one 1,1-dioxide

HRID 729266

반응식

HRID 729266 반응식
[Cl:1][C:2]1[C:3](=[O:15])[NH:4][S:5](=[O:14])(=[O:13])[C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.CI.[C:18](=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[Cl:1][C:2]1[C:3](=[O:15])[N:4]([CH3:18])[S:5](=[O:13])(=[O:14])[C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 68661656HCID 68661656, 화합물

생성물 1

HCID 686620174-Chloro-2-methyl-5-phenylisothiazol-3(2H)-one 1,1-dioxide수율 104%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide (2.0 g, 8.21 mmol) and MeI (3.5 g, 24.6 mmol) in DMF (30 ml) was cooled with an ice bath, and anhydrous potassium carbonate (1.13 g, 8.21 mmol) was added. The mixture was then allowed to warm to rt and stirred for 21 h. Water (60 ml) was added and the white precipitate formed, was filtered off and washed with water. Toluene was added to the precipitate and the mixture was evaporated and the residue was dried for three days under vacuum to give the title compound (2.2 g, 102%) containing traces of water and toluene. 1H NMR (400 MHz, CDCl3): δ 3.23 (s, 3H), 7.52-7.56 (m, 3H), 7.86-7.88 (m, 2H); 13C-NMR (100 MHz, CD3CN): δ 24.5, 123.8, 1291, 129.5, 130.7, 133.0, 143.1, 157.6.

후처리

  1. customthe white precipitate formed
  2. filtrationwas filtered off
  3. washwashed with water
  4. additionToluene was added to the precipitate
  5. customthe mixture was evaporated
  6. customthe residue was dried for three days under vacuum

출처 및 근거

ORD 기록
ord-45c600a773ac4635ba9a18c0d831f33a
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582629B2

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