Lithium borohydride → HCID 57785948, 화합물

HRID 1628706노트

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HRID 1628706 반응식
[BH4-].[Li+].[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([C:28](OC)=[O:29])=[C:8]2[C:12]=1[N:11]=[C:10]1[N:13]([C:17]3[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=3[C:24]([F:27])([F:26])[F:25])[CH2:14][CH2:15][CH2:16][N:9]21>O1CCCC1>[Cl:3][C:4]1[C:12]2[N:11]=[C:10]3[N:13]([C:17]4[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][C:18]=4[C:24]([F:26])([F:25])[F:27])[CH2:14][CH2:15][CH2:16][N:9]3[C:8]=2[C:7]([CH2:28][OH:29])=[CH:6][CH:5]=1

참가 물질

4

반응물 2

HCID 4148881Lithium borohydrideHCID 57785993HCID 57785993, 화합물

생성물 1

HCID 57785948HCID 57785948, 화합물수율 87%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

Lithium borohydride (2.14 g, 98.1 mmol) was added to a stirred solution of methyl 9-chloro-1-[4-chloro-2-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carboxylate (10.9 g, 24.5 mmol) in tetrahydrofuran (80 mL) at room temperature, and the mixture was stirred at room temperature for 12 hr and at 50° C. for 4 hr. The reaction was quenched by methanol, and the mixture was diluted with aqueous saturated ammonium chloride at 0° C. and 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 washed with ethyl acetate/diisopropyl ether to give the title compound as a colorless powder (8.81 g, 21.2 mmol, 87%).

후처리

  1. customThe reaction was quenched by methanol
  2. additionthe mixture was diluted with aqueous saturated ammonium chloride at 0° C.
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. washThe residue was washed with ethyl acetate/diisopropyl ether

출처 및 근거

ORD 기록
ord-0b03128708a842469e0de8df5e3e9b98
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785460B2

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