4-Toluenesulfonyl chloride → Benzyl 3-pyridyl ketone oxime p-toluenesulfonate

HRID 1462863노트

반응식

HRID 1462863 반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18](=[N:26][OH:27])[CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:13]=1>N1C=CC=CC=1>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([OH:27])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18](=[N:26][OH:27])[CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:13]=1

참가 물질

4

반응물 2

HCID 73974-Toluenesulfonyl chlorideHCID 72739677Benzyl 3-pyridyl ketone oxime

생성물 1

HCID 86739563Benzyl 3-pyridyl ketone oxime p-toluenesulfonate

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

A solution of 7.7 g of p-toluenesulfonyl chloride in 15 ml of pyridine is added dropwise in the course of 5 minutes to a solution, which is stirred at -10°, of 8.5 g of benzyl 3-pyridyl ketone oxime in 20 ml of pyridine. The reaction mixture is placed in a refrigerator for 24 hours and then poured onto ice/water. After some stirring and grinding, the oil which has separated out solidifies to crystals. These are filtered off with suction, washed with water and dried under a high vacuum. Benzyl 3-pyridyl ketone oxime p-toluenesulfonate is obtained and this is employed in the next stage without further purification.

후처리

  1. additionpoured onto ice/water
  2. customAfter some stirring and grinding
  3. customthe oil which has separated out solidifies to crystals
  4. filtrationThese are filtered off with suction
  5. washwashed with water
  6. customdried under a high vacuum

출처 및 근거

ORD 기록
ord-c9c035c0468048bfa730d0fd4e43619f
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461770

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