Methanol → HCID 68703601, 화합물

HRID 2244326노트

반응식

HRID 2244326 반응식
Cl[C:2]1(Cl)[CH2:4][C:3]1([C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1)[F:5].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+].CO>C1COCC1.C(OCC)(=O)C>[F:5][C:3]1([C:6]2[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=2)[CH2:2][CH2:4]1

참가 물질

7

반응물 4

HCID 887MethanolHCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydride2회HCID 687008961-(2,2-Dichloro-1-fluoro-cyclopropyl)-4-methyl-benzene

생성물 1

HCID 68703601HCID 68703601, 화합물수율 87%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

A solution of 1-(2,2-dichloro-1-fluoro-cyclopropyl)-4-methyl-benzene (1.18 g, 5.39 mmol) in THF (10 mL) was added at 0° C. to a suspension of lithium aluminum hydride (1.64 g, 43.1 mmol) in THF. The reaction mixture was stirred for 16 h at RT, then another portion of lithium aluminum hydride (613 mg, 16.1 mmol) was added, then after 3 h, 1 M aq. potassium sodium tartrate solution, methanol and ethyl acetate were added. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (SiO2, heptane) afforded the title compound (702 mg, 87%). Colourless liquid, MS (EI) 150.1 (M+).

후처리

  1. waitafter 3 h
  2. washThe organic layer was washed with brine
  3. dry with materialdried (MgSO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-d0014ce5ce7a4e52938c1bf911422fa0
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678818B2

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