Phosgene → Carbonochloridic acid, 2,4,5-trichlorophenyl ester

HRID 1376327ノート

反応式

HRID 1376327 の反応式
[C:1](Cl)([Cl:3])=[O:2].[Cl:5][C:6]1[CH:11]=[C:10]([Cl:12])[C:9]([Cl:13])=[CH:8][C:7]=1[OH:14].N1C2C(=CC=CC=2)C=CC=1>ClCCl>[Cl:3][C:1]([O:14][C:7]1[CH:8]=[C:9]([Cl:13])[C:10]([Cl:12])=[CH:11][C:6]=1[Cl:5])=[O:2]

参加物

5

反応物 3

HCID 6371Phosgene2 回HCID 7047QuinolineHCID 72712,4,5-Trichlorophenol

生成物 1

HCID 85650Carbonochloridic acid, 2,4,5-trichlorophenyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

About 7 g of phosgene are passed into a solution of 10.0 g of 2,4,5-trichlorophenol in 50 ml of dichloromethane at 0° C., and the mixture is stirred at 0° C. for 15 min. 7.2 ml of quinoline in 20 ml of dichloromethane are added dropwise over the course of 30 min, and the orange-colored suspension is then stirred in an ice bath for 1 h. Subsequently nitrogen is passed through the suspension for 1 h in order to blow out excess phosgene (absorber tower). The mixture is subsequently filtered, and the filtrate is washed twice with water, dried, again filtered and evaporated to dryness in vacuo. The 4.45 g of oily brownish residue are relatively pure 2,4,5-trichlorophenyl chloroformate, which crystallizes in the refrigerator and can be employed without further purification.

後処理

  1. stirringthe orange-colored suspension is then stirred in an ice bath for 1 h
  2. waitSubsequently nitrogen is passed through the suspension for 1 h in order
  3. filtrationThe mixture is subsequently filtered
  4. washthe filtrate is washed twice with water
  5. customdried
  6. filtrationagain filtered
  7. customevaporated to dryness in vacuo
  8. customcrystallizes in the refrigerator
  9. customcan be employed without further purification

出典と根拠

ORDレコード
ord-dae3b58bc3fc481baebdcff7e34f3ebc
出典データセット
uspto-grants-1997_09
特許番号
US05663141

反応ノート

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