Isopropyl Isothiocyanate → HCID 178456969、化合物

HRID 1066129

反応式

HRID 1066129 の反応式
[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

参加物

4

反応物 2

HCID 75263Isopropyl IsothiocyanateHCID 211978072-Amino-4-fluorobenzenesulfonamide

生成物 1

HCID 178456969HCID 178456969、化合物収率 14%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
140 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d22db6594ba8410e80d2b4b7b2d5dcdb
出典データセット
uspto-grants-2001_06
特許番号
US06242443B1

関連ノート

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