m-Aminoacetanilide → HCID 14476476、化合物

HRID 703923ノート

反応式

HRID 703923 の反応式
[C:1]([NH:4][C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][CH:11]=1)[NH2:8])(=[O:3])[CH3:2].C(N(CC)CC)C.[CH3:19][C:20]([CH3:25])=[CH:21][C:22](Cl)=[O:23]>ClCCl>[C:1]([NH:4][C:5]1[CH:11]=[CH:10][CH:9]=[C:7]([NH:8][C:22](=[O:23])[CH:21]=[C:20]([CH3:25])[CH3:19])[CH:6]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 7604m-AminoacetanilideHCID 8471TriethylamineHCID 1023943-Methyl-2-butenoyl chloride

生成物 1

HCID 14476476HCID 14476476、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

56.7 g. (0.42 mole) 3-acetamidoaniline in 400 ml. dichloromethane and 65 ml. (0.46 mol) triethylamine are mixed, while cooling with ice, with 59.0 g. (0.46 mole) 3,3-dimethylacryloyl chloride and stirred for 2 hours at ambient temperature. The solution is thereafter extracted with water and the separated organic phase is dried over anhydrous sodium sulphate, evaporated and the residue mixed with ethyl acetate. Upon standing in a refrigerator, crystals separate out. Yield 45.7 g. (47% of theory); m.p. 144°-148° C.

後処理

  1. temperaturewhile cooling with ice, with 59.0 g
  2. extractionThe solution is thereafter extracted with water
  3. dry with materialthe separated organic phase is dried over anhydrous sodium sulphate
  4. customevaporated
  5. additionthe residue mixed with ethyl acetate
  6. customseparate out

出典と根拠

ORDレコード
ord-5cf7946d7a114c4798439b7b990deb1a
出典データセット
uspto-grants-1991_01
特許番号
US04985448

反応ノート

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