Carbon Dioxide → 2-Chloro-4-fluoro-5-isothiocyanatothiobenzoic acid (methoxycarbonylmethyl) ester

HRID 1033216노트

반응식

HRID 1033216 반응식
[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[S:17])[C:8]1[CH:13]=[C:12]([NH2:14])[C:11]([F:15])=[CH:10][C:9]=1[Cl:16])=[O:4].C(=O)([O-])[O-].[Ca+2].[C:23](Cl)(Cl)=[S:24].C(=O)=O>ClCCl.O>[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[S:17])[C:8]1[CH:13]=[C:12]([N:14]=[C:23]=[S:24])[C:11]([F:15])=[CH:10][C:9]=1[Cl:16])=[O:4]

참가 물질

7

반응물 4

HCID 280Carbon DioxideHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 539902175-Amino-2-chloro-4-fluorothiobenzoic acid (methoxycarbonylmethyl) ester

생성물 1

HCID 538361362-Chloro-4-fluoro-5-isothiocyanatothiobenzoic acid (methoxycarbonylmethyl) ester

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3.8 g of the resulting 5-amino-2-chloro-4-fluorothiobenzoic acid (methoxycarbonylmethyl) ester in 100 ml of dichloromethane is added dropwise at from 25° to 30° C. to a suspension of 6 g of calcium carbonate, 4 ml of thiophosgene, 20 ml of dichloromethane and 20 ml of water. When the evolution of carbon dioxide has ceased, the batch is stirred for a further 18 hours at room temperature. After filtering and washing with water, the organic phase is separated off, dried over sodium sulfate and then concentrated by evaporation to yield 4.8 g of 2-chloro-4-fluoro-5-isothiocyanatothiobenzoic acid (methoxycarbonylmethyl) ester in the form of an oil which is used without further purification in the next reaction step.

후처리

  1. filtrationAfter filtering
  2. washwashing with water
  3. customthe organic phase is separated off
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-2b6338f223734276899fff354bb08cc9
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310722

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