Methanol → HCID 12046883、化合物

HRID 408141ノート

反応式

HRID 408141 の反応式
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]

参加物

4

反応物 3

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

生成物 1

HCID 12046883HCID 12046883、化合物収率 94%

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dd4e485d8cf14327b2368b18b9de5ffd
出典データセット
uspto-grants-2014_06
特許番号
US08758830B2

反応ノート

読み込み中…