Methanol → HCID 12046883, 화합물

HRID 1923669노트

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HRID 1923669 반응식
B(F)(F)F.[CH2:5]([O:7][P:8]([N:13]1[CH:19]2[CH:14]1[CH2:15][CH2:16][N:17]([C:20]([O:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[O:21])[CH2:18]2)([O:10][CH2:11][CH3:12])=[O:9])[CH3:6].[CH3:30][OH:31]>>[CH2:5]([O:7][P:8]([NH:13][C@H:19]1[C@H:14]([O:31][CH3:30])[CH2:15][CH2:16][N:17]([C:20]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:21])[CH2:18]1)([O:10][CH2:11][CH3:12])=[O:9])[CH3:6]

참가 물질

4

반응물 3

HCID 887MethanolHCID 6356Boron trifluorideHCID 59455678Benzyl 7-(diethoxyphosphoryl)-3,7-diazabicyclo[4.1.0]heptane-3-carboxylate

생성물 1

HCID 12046883HCID 12046883, 화합물수율 94%

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온도
0 °C

실험 절차

BF3 etherate (1.35 mL, 10.6 mmol) was added to a solution of benzyl 7-(diethoxyphosphoryl)-3,7-diazabicyclo[4.1.0]heptane-3-carboxylate (1.96 g, 5.32 mmol) in methanol (10 mL) at 0° C. and stirred at 0° C. for 2 hours. The solvent was removed in vacuo, ethyl acetate (30 mL) and saturated sodium bicarbonate (20 mL) were added. The organic layer was separated, dried (sodium sulfate) and concentrated in vacuo to give trans-benzyl 3-(diethoxyphosphorylamino)-4-methoxypiperidine-1-carboxylate (2.00 g, 94%) as an oil.

후처리

  1. customThe solvent was removed in vacuo, ethyl acetate (30 mL) and saturated sodium bicarbonate (20 mL)
  2. additionwere added
  3. customThe organic layer was separated
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-458e5d08e3e54a349855af2f38ae2885
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178131B2

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