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

HRID 1462863ノート

反応式

HRID 1462863 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 86739563Benzyl 3-pyridyl ketone oxime p-toluenesulfonate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c9c035c0468048bfa730d0fd4e43619f
出典データセット
uspto-grants-1984_07
特許番号
US04461770

反応ノート

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