Dichloromethane → HCID 14476476、化合物

HRID 1492164ノート

反応式

HRID 1492164 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].ClCCl.[CH3:15][C:16]([CH3:21])=[CH:17][C:18](Cl)=[O:19]>C(N(CC)CC)C>[C:1]([NH:4][C:5]1[CH:11]=[CH:10][CH:9]=[C:7]([NH:8][C:18](=[O:19])[CH:17]=[C:16]([CH3:21])[CH3:15])[CH:6]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 7604m-AminoacetanilideHCID 1023943-Methyl-2-butenoyl chloride

生成物 1

HCID 14476476HCID 14476476、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

56.7 g. ( 0.42 mole ) 3-acetamidoaniline in 400 ml. dichloromethane and 65 ml. ( 0.46 tool ) 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-63ae773b3cb74f3e97e5d7dbf6a30399
出典データセット
uspto-grants-1994_12
特許番号
US05373019

反応ノート

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