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Lithium borohydride → HCID 57785980, 화합물

HRID 1628716
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HRID 1628716 반응식
[BH4-].[Li+].[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([C:26](OC)=[O:27])=[C:8]2[C:12]=1[N:11]=[C:10]1[N:13]([C:17]3[C:22]([CH3:23])=[CH:21][C:20]([Cl:24])=[CH:19][C:18]=3[Cl: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[C:22]([CH3:23])=[CH:21][C:20]([Cl:24])=[CH:19][C:18]=4[Cl:25])[CH2:14][CH2:15][CH2:16][N:9]3[C:8]=2[C:7]([CH2:26][OH:27])=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4148881Lithium borohydrideHCID 57786000HCID 57786000, 화합물

생성물 1

HCID 57785980HCID 57785980, 화합물수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

Lithium borohydride (205 mg, 9.42 mmol) was added to a stirred solution of methyl 9-chloro-1-(2,4-dichloro-6-methylphenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole-6-carboxylate (800 mg, 1.88 mmol) in tetrahydrofuran (4.0 mL) at room temperature, and the mixture was stirred at 50° C. for 13 hr. The reaction was quenched by aqueous saturated ammonium chloride at 0° C. 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 washed with ethyl acetate/diisopropyl ether to give the title compound as a colorless powder (620 mg, 1.56 mmol, 83%).

후처리

  1. customThe reaction was quenched by aqueous saturated ammonium chloride at 0° C.
  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. washThe residue was washed with ethyl acetate/diisopropyl ether

출처 및 근거

ORD 기록
ord-4145e2bb57c549888419dec12e826ab5
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785460B2

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