Sodium Bicarbonate → HCID 59317181、化合物

HRID 389870ノート

反応式

HRID 389870 の反応式
[O:1]=[C:2]1[N:6]([CH3:7])[C:5]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)([CH2:8][O:9]CC=C)[C:4](=[O:19])[N:3]1[C:20]1[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[C:22]([C:28]([F:31])([F:30])[F:29])[CH:21]=1.C(=O)(O)[O-].[Na+]>ClCCl>[O:1]=[C:2]1[N:6]([CH3:7])[C:5]([CH2:8][OH:9])([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[C:4](=[O:19])[N:3]1[C:20]1[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[C:22]([C:28]([F:31])([F:29])[F:30])[CH:21]=1

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 67131041HCID 67131041、化合物

生成物 1

HCID 59317181HCID 59317181、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 0.52 g of 4-[2,5-dioxo-3-methyl-4-phenyl-4-[(2-propenyloxy)methyl]imidazolidin-1-yl]-2-trifluoromethylbenzonitrile in 40 mL of dichloromethane is added 2 mL of trifluoroborane-dimethylsulfide complex in 10 mL of dichloromethane. The mixture is stirred at rt for 3 hours and poured into a saturated aqueous sodium bicarbonate solution and extracted with ethyl acetate. The organic layer is dried over magnesium sulfate, filtered and evaporated. The crude product is purified by chromatography over silica gel while eluting with 70/30 heptane/ethyl acetate mixture to provide the desired product.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer is dried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude product is purified by chromatography over silica gel
  6. washwhile eluting with 70/30 heptane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-fb1f37ee52944df7b3f06dbf3786d65d
出典データセット
uspto-grants-2013_02
特許番号
US08383608B2

反応ノート

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