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

HRID 632020
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HRID 632020 반응식
[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
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참가 물질

5

반응물 3

HCID 887MethanolHCID 6331Borane2회HCID 64685110HCID 64685110, 화합물

생성물 1

HCID 595112562-Methyl-4-morpholinobutan-2-amine수율 17.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-05a0d710e1cc4b0d80df81d55b717d37
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321727B2

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