Trichloroacetyl chloride → 2-Trichloroacetylmethylene-3-ethyl-benzothiazoline

HRID 1089404

反応式

HRID 1089404 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[CH3:12][C:13]1[S:14][C:15]2[CH:23]=[CH:22][CH:21]=[CH:20][C:16]=2[N+:17]=1[CH2:18][CH3:19].C(N(CC)CC)C.[Cl:31][C:32]([Cl:37])([Cl:36])[C:33](Cl)=[O:34]>C1(C)C=CC=CC=1>[Cl:31][C:32]([Cl:37])([Cl:36])[C:33]([CH:12]=[C:13]1[N:17]([CH2:18][CH3:19])[C:16]2[CH:20]=[CH:21][CH:22]=[CH:23][C:15]=2[S:14]1)=[O:34]

参加物

5

反応物 3

HCID 6420Trichloroacetyl chlorideHCID 8471TriethylamineHCID 84711Benzothiazolium, 3-ethyl-2-methyl-, 4-methylbenzenesulfonate (1:1)

生成物 1

HCID 543960172-Trichloroacetylmethylene-3-ethyl-benzothiazoline

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

10 g (28.6 mmol) of 2-methyl-3-ethyl-benzothiazolium p-toluenesulfonate are suspended in 150 ml of toluene, 6.8 g (67.2 mmol) of triethylamine are added and, at 5°-10° C. 6 g (33 mmol) of trichloroacetyl chloride, dissolved in a minor amount of toluene, are added dropwise. After three hours at room temperature, the ammonium salts are filtered off with suction, and the reaction solution is washed with water, dried over sodium sulfate and concentrated in vacuo. The product is caused to crystallize from the diisopropyl ether.

後処理

  1. additionare added dropwise
  2. filtrationthe ammonium salts are filtered off with suction
  3. washthe reaction solution is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customto crystallize from the diisopropyl ether

出典と根拠

ORDレコード
ord-d6002d5007a34608ac0debe48ba35e09
出典データセット
uspto-grants-1990_10
特許番号
US04966828

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