tert-Butylacrylamide → HCID 14297377、化合物

HRID 845883

反応式

HRID 845883 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.CC(C)([O-])C.[K+].[C:23]([NH:27][C:28](=[O:31])[CH:29]=[CH2:30])([CH3:26])([CH3:25])[CH3:24]>O1CCCC1>[C:23]([NH:27][C:28](=[O:31])[CH2:29][CH2:30][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)([CH3:26])([CH3:25])[CH3:24]

参加物

5

反応物 3

HCID 7877tert-ButylacrylamideHCID 69297DibenzylhydroxylamineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 14297377HCID 14297377、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 21.33 g of dibenzylhydroxylamine in 100 ml of dry tetrahydrofuran is admixed with 1.12 g of potassium-tert-butoxide followed by 12.70 g of N-tert-butylacrylamide. The solution is heated under reflux for 24 hours under N2. The crude reaction mixture is concentrated under reduced pressure and the residue is partitioned between water and methylene chloride. The organic layer is washed with water, brine dried (MgSO4) and evaporated under reduced pressure. Purification by liquid chromatography affords the title compound as an oil.

後処理

  1. temperatureThe solution is heated
  2. temperatureunder reflux for 24 hours under N2
  3. customThe crude reaction mixture
  4. concentrationis concentrated under reduced pressure
  5. customthe residue is partitioned between water and methylene chloride
  6. washThe organic layer is washed with water, brine
  7. dry with materialdried (MgSO4)
  8. customevaporated under reduced pressure
  9. customPurification by liquid chromatography

出典と根拠

ORDレコード
ord-ae0ad8f5f7034c5786f95eee030825cc
出典データセット
uspto-grants-1988_07
特許番号
US04760179

関連ノート

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