Chloroacetyl chloride → 2-Chloro-N-[3,4-bis(phenylmethoxy)phenyl]acetamide

HRID 4112

반응식

HRID 4112 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:13]=[CH:14][C:15]=1[O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[NH2:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:24][CH2:25][C:26](Cl)=[O:27].C(=O)(O)[O-].[K+]>C(#N)C.O>[Cl:24][CH2:25][C:26]([NH:12][C:11]1[CH:13]=[CH:14][C:15]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:10]=1)=[O:27]

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chloride2회HCID 516893Potassium BicarbonateHCID 122537843,4-Dibenzyloxy aniline

생성물 1

HCID 201534662-Chloro-N-[3,4-bis(phenylmethoxy)phenyl]acetamide

시약·촉매·용매 1

HCID 18373917Acetonitrile--water (1/1)용매

실험 절차

To 7.7 g (25 mmol) of 3,4-dibenzyloxyaniline in 50 ml of 1:1 acetonitrile/water at 0° C. was added chloroacetyl chloride (3.0 ml) while keeping the pH at 6.5 with saturated aqueous potassium bicarbonate. When the pH remained constant for 15 minutes, an additional 3 ml of chloroacetyl chloride was added in small portions while maintaining the pH at 6.5. When the pH remained constant for 15 minutes, the acetonitrile was evaporated, and the resulting aqueous solution was filtered. The precipitate was washed thoroughly with water to yield, upon drying in vacuo, 8.98 g of the title compound.

후처리

  1. temperaturewhile maintaining the pH at 6.5
  2. waitWhen the pH remained constant for 15 minutes
  3. customthe acetonitrile was evaporated
  4. filtrationthe resulting aqueous solution was filtered
  5. washThe precipitate was washed thoroughly with water
  6. customto yield
  7. dry with materialupon drying in vacuo, 8.98 g of the title compound

출처 및 근거

ORD 기록
ord-b9d7e217a7e7454187283988eab03121
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723002

연결된 노트

불러오는 중…