Benzocaine → 4-(p-Methoxycinnamamido)benzoic acid, ethyl ester

HRID 485251

反応式

HRID 485251 の反応式
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]([CH:7]=[CH:8][C:9](Cl)=[O:10])=[CH:5][CH:4]=1.[CH3:14][CH2:15][O:16][C:17]([C:19]1[CH:20]=[CH:21][C:22]([NH2:25])=[CH:23][CH:24]=1)=[O:18].C(N(CC)CC)C>ClCCl>[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]([CH:7]=[CH:8][C:9]([NH:25][C:22]2[CH:21]=[CH:20][C:19]([C:17]([O:16][CH2:15][CH3:14])=[O:18])=[CH:24][CH:23]=2)=[O:10])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 2337BenzocaineHCID 8471TriethylamineHCID 534017724-Methoxycinnamic acid chloride

生成物 1

HCID 7072084-(p-Methoxycinnamamido)benzoic acid, ethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 10 g. of p-methoxycinnamoyl chloride in 200 ml. of dichloromethane is slowly added a solution of 0.24 g. of benzocaine and 7.1 ml. of triethylamine in 200 ml. of dichloromethane. The mixture is stirred for 19 hours, then the organic layer is washed with 200 ml. of 10% hydrochloric acid followed by 200 ml. of brine, dried over magnesium sulfate, and condensed to a solid. This solid is crystallized from 100 ml. of ethanol, giving 10.6 g. of the desired product as yellow crystals, m.p. 163°-165.5° C.

後処理

  1. washthe organic layer is washed with 200 ml
  2. dry with materialof brine, dried over magnesium sulfate, and condensed to a solid
  3. customThis solid is crystallized from 100 ml
  4. customof ethanol, giving 10.6 g

出典と根拠

ORDレコード
ord-872c52fc9c8a4b789856800578381588
出典データセット
uspto-grants-1985_08
特許番号
US04536346

関連ノート

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