Dimethylsulphamoyl chloride → HCID 54319481, 화합물

HRID 1287846노트

반응식

HRID 1287846 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 54319481HCID 54319481, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0fd166a0ff4f4d43964d065de08ba4fc
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03985887

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