Triethylamine → Ethyl-beta-methanesulfonylamino-beta-ethoxy Acrylate

HRID 1449070ノート

反応式

HRID 1449070 の反応式
[C:1]([O:5][O:6][C:7]([CH2:10][CH3:11])([NH2:9])[CH3:8])(=[O:4])[CH:2]=[CH2:3].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>C1C=CC=CC=1>[C:1]([O:5][O:6][C:7]([CH2:10][CH3:11])([NH:9][S:20]([CH3:19])(=[O:22])=[O:21])[CH3:8])(=[O:4])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86736826Ethylbeta-amino-beta-ethoxy acrylate

生成物 1

HCID 86736825Ethyl-beta-methanesulfonylamino-beta-ethoxy Acrylate収率 67.5%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a solution of 15.9 g of ethyl-β-amino-β-ethoxy acrylate in 60 ml of benzene was added 10.3 g of triethylamine, and a solution of 11.5 g of methanesulfonyl chloride in 40 ml of benzene was dropped thereinto with stirring. After the dropping, the resulting mixture was stirred at room temperature for 5 hours. The crystals formed were separated. The filtrate was concentrated under reduced pressure and the concentrated residue crystallized by cooling. When the crystals were washed with n-hexane and dried, 16 g of prismatic crystals of a melting point of 103° to 104° C. was obtained.

後処理

  1. stirringAfter the dropping, the resulting mixture was stirred at room temperature for 5 hours
  2. customThe crystals formed
  3. customwere separated
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe concentrated residue crystallized
  6. temperatureby cooling
  7. washWhen the crystals were washed with n-hexane
  8. customdried

出典と根拠

ORDレコード
ord-839034f6a2784c26b0bd820fc693f70b
出典データセット
uspto-grants-1980_02
特許番号
US04188489

反応ノート

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