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Potassium Carbonate → HCID 21999985、化合物

HRID 1975930
ノート
印刷プレビュー

反応式

HRID 1975930 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:11])[C:6]=1[S:7]([NH2:10])(=[O:9])=[O:8].C(=O)([O-])[O-].[K+].[K+].[CH:18]([N:21]=[C:22]=[S:23])([CH3:20])[CH3:19]>CC(C)=O>[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH3:11])[C:6]=1[S:7]([NH:10][C:22]([NH:21][CH:18]([CH3:20])[CH3:19])=[S:23])(=[O:8])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 75263Isopropyl IsothiocyanateHCID 21999992HCID 21999992、化合物

生成物 1

HCID 21999985HCID 21999985、化合物収率 54%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
52.5 °C

実験手順

A mixture of 2-amino-4-methyl-thiophene-3-sulfonamide (0.30 g), potassium carbonate (0.32 g), and isopropyl isothiocyanate (272 μl) in dry acetone (5 ml) under nitrogen was heated at 50-55° C. overnight. Then the solvent was evaporated and the residue was dissolved in water (15 ml); pH was adjusted to 2 by addition of 4 M hydrochloric acid, and the mixture was stirred for 30 min. The precipitated crystals were filtered off, rinsed with a small amount of water and dried to give 0.24 g (yield 54%) of the title compound; m.p. 118-120° C.

後処理

  1. customThen the solvent was evaporated
  2. dissolutionthe residue was dissolved in water (15 ml)
  3. additionpH was adjusted to 2 by addition of 4 M hydrochloric acid
  4. filtrationThe precipitated crystals were filtered off
  5. washrinsed with a small amount of water
  6. customdried

出典と根拠

ORDレコード
ord-4e2b7c729df241509aa68d30473bd481
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06225310B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート