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Thiophosgene → 1-(2-Chloro-4-fluoro-5-isothiocyanato-phenylthio)-cyclopropanecarboxylic acid methyl ester

HRID 1646467
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반응식

HRID 1646467 반응식
[CH3:1][O:2][C:3]([C:5]1([S:8][C:9]2[CH:14]=[C:13]([NH2:15])[C:12]([F:16])=[CH:11][C:10]=2[Cl:17])[CH2:7][CH2:6]1)=[O:4].C(=O)([O-])[O-].[Ca+2].[C:23](Cl)(Cl)=[S:24]>C(Cl)CCl.O>[CH3:1][O:2][C:3]([C:5]1([S:8][C:9]2[CH:14]=[C:13]([N:15]=[C:23]=[S:24])[C:12]([F:16])=[CH:11][C:10]=2[Cl:17])[CH2:7][CH2:6]1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 54364994HCID 54364994, 화합물

생성물 1

HCID 545373801-(2-Chloro-4-fluoro-5-isothiocyanato-phenylthio)-cyclopropanecarboxylic acid methyl ester

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매2회HCID 962Water
용매

실험 절차

While stirring at room temperature, a solution of 5.5 g of 1-(5-amino-2-chloro-4-fluoro-phenylthio)-cyclopropanecarboxylic acid methyl ester in 20 ml of ethylene chloride is added dropwise to a mixture of 3 g of calcium carbonate, 2 ml of thiophosgene in 20 ml of ethylene chloride and 20 ml of water. After stirring for 4 hours at room temperature, the inorganic portion of the reaction mixture is filtered off and the organic phase is dried over calcium chloride and then concentrated by evaporation, yielding 6.3 g of 1-(2-chloro-4-fluoro-5-isothiocyanato-phenylthio)-cyclopropanecarboxylic acid methyl ester having a melting point of from +100° to +101° C.

후처리

  1. stirringAfter stirring for 4 hours at room temperature
  2. filtrationthe inorganic portion of the reaction mixture is filtered off
  3. dry with materialthe organic phase is dried over calcium chloride
  4. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-f5712137e94243649ca02083702274cb
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05180418

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