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

HRID 846015
ノート
印刷プレビュー

反応式

HRID 846015 の反応式
[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[O:22])[C:8]1[C:13]([C:14]2([Cl:21])[CH2:18][C:17]([F:19])=[C:16]([NH2:20])[S:15]2)=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:4].C(=O)([O-])[O-].[Ca+2].[C:28](Cl)(Cl)=[S:29].C(=O)=O>ClCCl.O>[CH3:1][O:2][C:3]([CH2:5][O:6][C:7](=[O:22])[C:8]1[C:13]([C:14]2([Cl:21])[CH2:18][C:17]([F:19])=[C:16]([N:20]=[C:28]=[S:29])[S:15]2)=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 280Carbon DioxideHCID 10040ThiophosgeneHCID 10112Calcium CarbonateHCID 867460235-Amino-2-chloro-4-fluoro-thiolbenzoic acid (methoxycarbonylmethyl) ester

生成物 1

HCID 867460252-Chloro-4-fluoro-5-isothiocyanato-thiolbenzoic acid (methoxycarbonylmethyl) ester

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 3.8 g of the 5-amino-2-chloro-4-fluoro-thiolbenzoic acid (methoxycarbonylmethyl) ester obtained in accordance with Example P2 in 100 ml of dichloromethane is added dropwise at 25°-30° C. to a suspension of 6 g of calcium carbonate, 4 ml of thiophosgene, 20 ml of dichloromethane and 20 ml of water. After the evolution of carbon dioxide has ceased, the mixture is stirred for 18 hours at room temperature. After filtration and washing with water, the organic phase is separated off, dried over sodium sulfate and then concentrated by evaporation, yielding 4.8 g of 2-chloro-4-fluoro-5-isothiocyanato-thiolbenzoic acid (methoxycarbonylmethyl) ester in the form of an oil which is used in the next reaction step without further purification.

後処理

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

出典と根拠

ORDレコード
ord-8ca9c1d976dc4be191799f94c561a7dc
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05135562

反応ノート

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