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

HRID 1089404

반응식

HRID 1089404 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 543960172-Trichloroacetylmethylene-3-ethyl-benzothiazoline

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6002d5007a34608ac0debe48ba35e09
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04966828

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