Water → Methyl 4-benzyl-3-methylmorpholine-3-carboxylate

HRID 1696000ノート

反応式

HRID 1696000 の反応式
[CH2:1]([N:8]1[C:13](=O)[CH2:12][O:11][CH2:10][C:9]1([CH3:19])[C:15]([O:17][CH3:18])=[O:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.CCOC(C)=O>C1COCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][O:11][CH2:10][C:9]1([CH3:19])[C:15]([O:17][CH3:18])=[O:16])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 962WaterHCID 8857Ethyl AcetateHCID 67268468Methyl 4-benzyl-3-methyl-5-oxomorpholine-3-carboxylate

生成物 1

HCID 67268304Methyl 4-benzyl-3-methylmorpholine-3-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Dissolve methyl 4-benzyl-3-methyl-5-oxomorpholine-3-carboxylate in THF (10 volumes) and cool to 0° C. Add borane dimethylsulfide complex (1.5 eq) and allow to warm to room temperature. Add water (5 volumes) followed by EtOAc (10 volumes). Separate the organic layer, wash with saturated aqueous NaCl, dry over sodium sulfate, filtered, and concentrate to give methyl 4-benzyl-3-methylmorpholine-3-carboxylate.

後処理

  1. temperatureto warm to room temperature
  2. customSeparate the organic layer
  3. washwash with saturated aqueous NaCl
  4. dry with materialdry over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrate

出典と根拠

ORDレコード
ord-d21651bcb7a1415daf402a3a26ea931d
出典データセット
uspto-grants-2012_04
特許番号
US08163755B2

反応ノート

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