p-(p-Chlorocinnamamido)benzoic acid, ethyl ester → HCID 13503432、化合物

HRID 485248ノート

反応式

HRID 485248 の反応式
[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH:6]=[CH:7][C:8]([NH:10][C:11]2[CH:21]=[CH:20][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:13][CH:12]=2)=[O:9])=[CH:4][CH:3]=1.[H][H]>[Pd].O1CCCC1>[Cl:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][CH2:7][C:8]([NH:10][C:11]2[CH:12]=[CH:13][C:14]([C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:20][CH:21]=2)=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 2

HCID 692488p-(p-Chlorocinnamamido)benzoic acid, ethyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 13503432HCID 13503432、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 30.0 g. of 4-(p-chlorocinnamamido)benzoic acid, ethyl ester, 500 mg. of 10% palladium on carbon, and 150 ml. of tetrahydrofuran is hydrogenated in a Parr apparatus, over a 2 hour period, repressurizing until hydrogen uptake is complete. The mixture is filtered, and the filtrate is evaporated. The solid is crystallized from 175 ml. of ethanol, giving 26.8 g. of the desired product as white crystals, m.p. 163°-165° C.

後処理

  1. additionA mixture of 30.0 g
  2. filtrationThe mixture is filtered
  3. customthe filtrate is evaporated
  4. customThe solid is crystallized from 175 ml
  5. customof ethanol, giving 26.8 g

出典と根拠

ORDレコード
ord-3faf2a09773d453fb8666c6fc6dcaa3f
出典データセット
uspto-grants-1985_08
特許番号
US04536346

反応ノート

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