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

HRID 4112

反応式

HRID 4112 の反応式
[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]

参加物

5

反応物 3

HCID 6577Chloroacetyl chloride2 回HCID 516893Potassium BicarbonateHCID 122537843,4-Dibenzyloxy aniline

生成物 1

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

試薬・触媒・溶媒 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b9d7e217a7e7454187283988eab03121
出典データセット
uspto-grants-1988_02
特許番号
US04723002

関連ノート

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