Isopropyl Isothiocyanate → HCID 178456969, 화합물

HRID 1066129

반응식

HRID 1066129 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10].[CH:13]([N:16]=[C:17]=S)([CH3:15])[CH3:14]>C(OCC)(=O)C>[F:8][C:6]1[CH:5]=[CH:4][C:3]2[S:9](=[O:11])(=[O:10])[N:12]=[C:17]([NH:16][CH:13]([CH3:15])[CH3:14])[NH:1][C:2]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 75263Isopropyl IsothiocyanateHCID 211978072-Amino-4-fluorobenzenesulfonamide

생성물 1

HCID 178456969HCID 178456969, 화합물수율 14%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
140 °C

실험 절차

A mixture of 2-amino-4-fluorobenzenesulfonamide (1.9 g, 10 mmol) and isopropyl isothiocyanate (6.4 ml, 60 mmol) was heated at 140° C. for 2.5 h. The mixture was cooled to room temperature and stirred with 50 ml of ethyl acetate for 20 min. The precipitate was isolated by filtration and washed with ethyl acetate to give 355 mg (14%) of the title compound; m.p. 266-269° C.; 1H-NMR (DMSO-d6): δ 1.18 (d, 6H, CH(CH3)2), 3.91 (m, 1H, CH(CH3)2), 7.00-7.13 (m, 2H, ArH), 7.16 (br.s, 1H, NH), 7.73 (dd, 1H, ArH), 10.4 (br.s, 1H, NH); MS: m/e 257 (M+, 25%); (C10H12N3F1O2S1) calc. C, 46.68; H, 4.70; N, 16.33; found C, 46.84; H, 4.88; N, 16.13.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. customThe precipitate was isolated by filtration
  3. washwashed with ethyl acetate

출처 및 근거

ORD 기록
ord-d22db6594ba8410e80d2b4b7b2d5dcdb
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242443B1

연결된 노트

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