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

HRID 417945

反応式

HRID 417945 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-752a22679006497f8d1083d89e310ac5
出典データセット
uspto-grants-2012_01
特許番号
US08093248B2

関連ノート

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