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

HRID 1376327

반응식

HRID 1376327 반응식
[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]

참가 물질

5

반응물 3

HCID 6371Phosgene2회HCID 7047QuinolineHCID 72712,4,5-Trichlorophenol

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dae3b58bc3fc481baebdcff7e34f3ebc
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663141

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