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Acetone → Bis(2-chloro-4-fluoro-5-methoxycarbonylaminophenyl)carbonate

HRID 1198779
ノート
印刷プレビュー

反応式

HRID 1198779 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH2:9])=[CH:4][C:3]=1[O:10][C:11](=[O:22])[O:12][C:13]1[CH:18]=[C:17]([NH2:19])[C:16]([F:20])=[CH:15][C:14]=1[Cl:21].[C:23](=[O:26])([O-:25])[O-].[K+].[K+].Cl[C:30]([O:32][CH3:33])=[O:31].[CH3:34]C(C)=O>>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH:9][C:23]([O:25][CH3:34])=[O:26])=[CH:4][C:3]=1[O:10][C:11](=[O:22])[O:12][C:13]1[CH:18]=[C:17]([NH:19][C:30]([O:32][CH3:33])=[O:31])[C:16]([F:20])=[CH:15][C:14]=1[Cl:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 180Acetone2 回HCID 6586Methyl chloroformateHCID 11430Potassium CarbonateHCID 15766649Bis(2-chloro-4-fluoro-5-aminophenyl)carbonate

生成物 1

HCID 15766844Bis(2-chloro-4-fluoro-5-methoxycarbonylaminophenyl)carbonate収率 88.2%

反応条件

温度
60 °C

実験手順

Dry acetone (1500 ml) was added to a mixture comprising bis(2-chloro-4-fluoro-5-aminophenyl)carbonate (233 g, 0.68 mol) and potassium carbonate (188 g, 1.36 mol), and methyl chloroformate (126 g, 1.33 mol) was dropwise added to the resulting solution, and the mixture was heated at 60° C. for 4 hours with stirring. After reaction, acetone was removed by distillation under reduced pressure, acetic acid was added so that the reaction mixture was made acidic, and thereafter the acidic mixture was poured into ice-water. The solid as precipitated out was taken out by filtration, washed with water and fully dried to obtain a white solid of bis(2-chloro-4-fluoro-5-methoxycarbonylaminophenyl)carbonate (279 g, 0.60 mol). Yield: 88.2 %. Spectral data and other data of the product are those as shown in Example 11.

後処理

  1. additionwas dropwise added to the resulting solution
  2. customwas removed by distillation under reduced pressure, acetic acid
  3. additionwas added so that the reaction mixture
  4. additionthe acidic mixture was poured into ice-water
  5. customThe solid as precipitated
  6. filtrationout was taken out by filtration
  7. washwashed with water
  8. customfully dried

出典と根拠

ORDレコード
ord-cf826350dcfb48d89d3f42f92d5ff832
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05281742

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート