4-Methylmorpholine → (1-Methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate

HRID 417945

반응식

HRID 417945 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([CH2:8][OH:9])[CH2:4][CH2:3]1.[N+:10]([C:13]1[CH:18]=[CH:17][C:16]([O:19][C:20](=O)[O:21]C2C=CC([N+]([O-])=O)=CC=2)=[CH:15][CH:14]=1)([O-:12])=[O:11].CN1CCOCC1>C(Cl)Cl>[C:20](=[O:21])([O:19][C:16]1[CH:15]=[CH:14][C:13]([N+:10]([O-:12])=[O:11])=[CH:18][CH:17]=1)[O:9][CH2:8][CH:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1

참가 물질

5

반응물 3

HCID 79724-MethylmorpholineHCID 78756Bis(4-nitrophenyl) carbonateHCID 2719711-Methyl-4-piperidinemethanol

생성물 1

HCID 57445006(1-Methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate수율 73.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

(1-Methylpiperidin-4-yl)methanol (2.50 g, 19.3 mmol) in DCM (50 mL) was added to a solution of bis-(4-nitrophenyl)carbonate (7.06 g, 23.2 mmol) in DCM (100 mL), followed by NMM (1.70 mL, 15.5 mmol). The reaction mixture was stirred for 90 hours and then washed sequentially with aliquots of 1 M aq Na2CO3 solution until the aqueous layer was colourless. The organic layer was dried (MgSO4) and concentrated in vacuo to give (1-methylpiperidin-4-yl)methyl 4-nitrophenyl carbonate (4.18 g, 73%) as a yellow solid.

후처리

  1. washwashed sequentially with aliquots of 1 M aq Na2CO3 solution until the aqueous layer
  2. dry with materialThe organic layer was dried (MgSO4)
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-752a22679006497f8d1083d89e310ac5
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093248B2

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