Methyl Acrylate → HCID 21621270、化合物

HRID 979258ノート

反応式

HRID 979258 の反応式
[CH2:1]([N:8]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[OH:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17]([O:21][CH3:22])(=[O:20])[CH:18]=[CH2:19].CC(C)([O-])C.[K+]>O1CCCC1>[CH3:22][O:21][C:17](=[O:20])[CH2:18][CH2:19][O:9][N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 7294Methyl AcrylateHCID 69297DibenzylhydroxylamineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 21621270HCID 21621270、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 42.6 g of N,N-dibenzylhydroxylamine, 25.8 g of methyl acrylate and 2.0 g of potassium-tert-butoxide in 200 ml of tetrahydrofuran is heated under reflux for 12 hours under N2. The crude reaction mixture is concentrated under reduced pressure and the residue is partitioned between water and ether. The orcanic layer is washed with water, saturated NaHSO4 solution and brine, dried (MgSO4) and then evaporated under reduced pressure to give the title compound as an oil.

後処理

  1. temperatureunder reflux for 12 hours under N2
  2. customThe crude reaction mixture
  3. concentrationis concentrated under reduced pressure
  4. customthe residue is partitioned between water and ether
  5. washThe orcanic layer is washed with water, saturated NaHSO4 solution and brine
  6. dry with materialdried (MgSO4)
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-55086bda318e429d99808034e1a1d662
出典データセット
uspto-grants-1987_05
特許番号
US04666962

反応ノート

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