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Methanol → 2-Methyl-4-morpholinobutan-2-amine

HRID 927406
ノート
印刷プレビュー

反応式

HRID 927406 の反応式
[NH2:1][C:2]([CH3:13])([CH3:12])[CH2:3][C:4]([N:6]1[CH2:11][CH2:10][O:9][CH2:8][CH2:7]1)=O.B.CO>C1COCC1>[CH3:13][C:2]([NH2:1])([CH3:12])[CH2:3][CH2:4][N:6]1[CH2:7][CH2:8][O:9][CH2:10][CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 6331Borane2 回HCID 64685110HCID 64685110、化合物

生成物 1

HCID 595112562-Methyl-4-morpholinobutan-2-amine収率 17.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

3-Amino-3-methyl-1-morpholinobutan-1-one (0.55 g, 2.96 mmol) and borane in THF (1 M, 6 mL, 6 mmol) were mixed together. The mixture was stirred at room temperature overnight, another portion borane in THF (6 mL) was added and the mixture stirred for another day. Methanol (5 mL) was added and the solvent was removed in vacuo. Water (20 mL) was added and the mixture was extracted with ethyl acetate (3×20 mL). The LC-MS showed still product in the water phase which was now extracted with methylene chloride (2×20 mL). The organic phases were combined, dried over anhydrous sodium sulfate and the solvent was removed in vacuo to give the crude product (0.09 g); MS (EI): m/e=173.2 [M+H]+.

後処理

  1. stirringthe mixture stirred for another day
  2. customthe solvent was removed in vacuo
  3. additionWater (20 mL) was added
  4. extractionthe mixture was extracted with ethyl acetate (3×20 mL)
  5. extractionwas now extracted with methylene chloride (2×20 mL)
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-4943f3b5706449bd9914a341b2f33dc4
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290451B2

反応ノート

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