HCID 57785864、化合物 → HCID 57786162、化合物

HRID 1628711ノート

反応式

HRID 1628711 の反応式
[CH2:1]([Mg]Br)[CH3:2].[Cl:5][C:6]1[CH:7]=[CH:8][C:9]([CH:30]=[O:31])=[C:10]2[C:14]=1[N:13]=[C:12]1[N:15]([C:19]3[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=3[C:26]([F:29])([F:28])[F:27])[CH2:16][CH2:17][CH2:18][N:11]21>O1CCCC1>[Cl:5][C:6]1[C:14]2[N:13]=[C:12]3[N:15]([C:19]4[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][C:20]=4[C:26]([F:28])([F:27])[F:29])[CH2:16][CH2:17][CH2:18][N:11]3[C:10]=2[C:9]([CH:30]([OH:31])[CH2:1][CH3:2])=[CH:8][CH:7]=1

参加物

4

反応物 2

HCID 57785864HCID 57785864、化合物HCID 178418443HCID 178418443、化合物

生成物 1

HCID 57786162HCID 57786162、化合物収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethylmagnesium bromide (3.0 M solution in diethyl ether, 0.35 mL, 1.05 mmol) was added to a stirred solution of 9-chloro-1-[4-chloro-2-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carbaldehyde (400 mg, 0.966 mmol) in tetrahydrofuran (3.0 mL) at 0° C., and the mixture was stirred at room temperature for 1 hr. The reaction was quenched by water, and the mixture was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue was recrystallized from ethanol to give the title compound as a colorless crystal (411 mg, 0.925 mmol, 96%).

後処理

  1. customThe reaction was quenched by water
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-6385ce0232bf4b33bf2ee429e89fa30e
出典データセット
uspto-grants-2014_07
特許番号
US08785460B2

反応ノート

読み込み中…