HCID 57785864、化合物 → HCID 57786345、化合物

HRID 1399065ノート

反応式

HRID 1399065 の反応式
[CH:1]1([Mg]Br)[CH2:3][CH2:2]1.[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([CH:31]=[O:32])=[C:11]2[C:15]=1[N:14]=[C:13]1[N:16]([C:20]3[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=3[C:27]([F:30])([F:29])[F:28])[CH2:17][CH2:18][CH2:19][N:12]21>O1CCCC1>[Cl:6][C:7]1[C:15]2[N:14]=[C:13]3[N:16]([C:20]4[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][C:21]=4[C:27]([F:28])([F:30])[F:29])[CH2:17][CH2:18][CH2:19][N:12]3[C:11]=2[C:10]([CH:31]([CH:1]2[CH2:3][CH2:2]2)[OH:32])=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 57785864HCID 57785864、化合物HCID 178418630HCID 178418630、化合物

生成物 1

HCID 57786345HCID 57786345、化合物収率 51.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Cyclopropylmagnesium bromide (1.0 M solution in tetrahydrofuran, 2.9 mL, 2.9 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 (1.00 g, 2.41 mmol) in tetrahydrofuran (10 mL) at 0° C., and the mixture was stirred at room temperature for 1 hr. The reaction was quenched by aqueous saturated ammonium chloride, 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 ethyl acetate to give the title compound as a colorless crystal (567 mg, 1.24 mmol, 51%).

後処理

  1. customThe reaction was quenched by aqueous saturated ammonium chloride
  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 ethyl acetate

出典と根拠

ORDレコード
ord-5f0869e0ac9f4566838c643173c4eeaa
出典データセット
uspto-grants-2014_12
特許番号
US08901141B2

反応ノート

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