Isobutyl isothiocyanate → HCID 178448905, 화합물

HRID 1066126

반응식

HRID 1066126 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10].[CH2:13]([N:17]=[C:18]=S)[CH:14]([CH3:16])[CH3:15]>C(OCC)(=O)C>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]2[S:9](=[O:11])(=[O:10])[N:12]=[C:18]([NH:17][CH2:13][CH:14]([CH3:16])[CH3:15])[NH:1][C:2]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 68960Isobutyl isothiocyanateHCID 777902-Amino-4-chlorobenzenesulphonamide

생성물 1

HCID 178448905HCID 178448905, 화합물수율 42%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
150 °C

실험 절차

A mixture of 2-amino-4-chlorobenzenesulfonamide (5.0 g, 24.18 mmol) and isobutyl isothiocyanate (10 ml, 83.6 mmol) was heated at 150° C. for 3 h. The mixture was allowed to cool and then stirred with 50 ml of ethyl acetate for 30 min. The precipitate was isolated by filtration and recrystallised from ethanol to give 2.9 g (42%) of the pure title compound; m.p. 298-301° C.; 1H-NMR (DMSO-d6): δ 0.91 (d, 6H, CH(CH3)2), 1.83 (m, 1H, CH(CH3)2), 3.05 (t, 2H, CH2), 7.2-7.4 (m, 3H, ArH+NH), 7.67 (d, 1H, ArH), 10.5 (br.s, 1H, NH); MS: m/e 287/289 (M+); (C11H14N3Cl1O2S1) calc. C, 45.91; H, 4.90; N, 14.60; found C, 45.90; H, 5.04; N, 14.66.

후처리

  1. temperatureto cool
  2. customThe precipitate was isolated by filtration
  3. customrecrystallised from ethanol

출처 및 근거

ORD 기록
ord-ee324be6274f4edaa8faeee3e26acfe8
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242443B1

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