Boron trifluoride etherate → HCID 15158051、化合物

HRID 1650723ノート

反応式

HRID 1650723 の反応式
[CH:1]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])OCC.B(F)(F)F.CCOCC.[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[C:26](=[O:34])[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=1.C(N(C(C)C)CC)(C)C.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[CH2:9]([O:8][CH:1]([O:5][CH2:6][CH3:7])[CH:27]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][N:29]=1)[C:26]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][N:20]=1)=[O:34])[CH3:10]

参加物

8

反応物 5

HCID 8000Boron trifluoride etherateHCID 31214Ethyl orthoformateHCID 81531DiisopropylethylamineHCID 2384361,2-di(pyridin-2-yl)ethanoneHCID 516892Sodium Bicarbonate

生成物 1

HCID 15158051HCID 15158051、化合物収率 141.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of 15 mL (0.089 mol) of triethyl orthoformate in 100 mL of methylene chloride was stirred under nitrogen at -78° C. and 13.2 mL (0.108 mol) of boron trifluoride etherate was added. The solution was allowed to warm to 0° C., recooled to -78° C., and a solution of 8.0 g (0.04 mol) of 1.2-bis(2-pyridinyl)ethanone in 75 mL of methylene chloride was added, followed after 30 min by 22 mL (0.132 mol) of diisopropylethylamine in 30 mL of methylene chloride. The reaction was stirred 45 min at -78° C., poured into 400 mL of water containing 10 g of NaHCO3 and stirred 20 min. The phases were separated, the methylene chloride layer was dried over MgSO4 and stripped to yield about 17 g of crude 3,3-diethoxy-1,2-bis(2-pyridinyl)-1-propanone.

後処理

  1. customrecooled to -78° C.
  2. stirringstirred 20 min
  3. customThe phases were separated
  4. dry with materialthe methylene chloride layer was dried over MgSO4

出典と根拠

ORDレコード
ord-1aae487049d244c182c83ceb84504e62
出典データセット
uspto-grants-1990_05
特許番号
US04925857

反応ノート

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