Dimethylsulphamoyl chloride → HCID 54319481、化合物

HRID 1287846ノート

反応式

HRID 1287846 の反応式
[CH3:1][N:2]([CH3:7])[S:3](Cl)(=[O:5])=[O:4].[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[C:18]([NH2:30])[CH:17]=1)=[O:15]>N1C=CC=CC=1.O>[N:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)=[C:18]([NH:30][S:3](=[O:5])(=[O:4])[N:2]([CH3:7])[CH3:1])[CH:17]=1)=[O:15]

参加物

5

反応物 2

HCID 83372Dimethylsulphamoyl chlorideHCID 538809743-Amino-4-benzyloxyphenyl 2-pyridyl ketone

生成物 1

HCID 54319481HCID 54319481、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒2 回

実験手順

A solution of 4.7 g (32.8 mmol) of dimethylsulfamyl chloride in 5 ml of dry pyridine is added to 5.0 g (16.4 mmol) of 3-amino-4-benzyloxyphenyl 2-pyridyl ketone in 100 ml of dry pyridine at 0°-10° C. The reaction mixture is stirred in the cold overnight and then poured in water and extracted with ether. The ether extract is washed with water and extracted with dilute aqueous KOH. This basic extract is washed with ether, acidified with hydrochloric acid and extracted with methylene chloride. The dried organic extract is evaporated in vacuo to give 4-benzyloxy-3-dimethylsulfamoylaminophenyl 2-pyridyl ketone. Hydrogenation over PcO2 according to the procedure of Example 3 gives α-(4-hydroxy-3-dimethylsulfamoylaminophenyl)-2-piperidylcarbinol.

後処理

  1. extractionextracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. extractionextracted with dilute aqueous KOH
  5. extractionThis basic extract
  6. washis washed with ether
  7. extractionextracted with methylene chloride
  8. extractionThe dried organic extract
  9. customis evaporated in vacuo

出典と根拠

ORDレコード
ord-0fd166a0ff4f4d43964d065de08ba4fc
出典データセット
uspto-grants-1976_10
特許番号
US03985887

反応ノート

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