Methanol → HCID 68703601、化合物

HRID 2244326ノート

反応式

HRID 2244326 の反応式
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

参加物

7

反応物 4

HCID 887MethanolHCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydride2 回HCID 687008961-(2,2-Dichloro-1-fluoro-cyclopropyl)-4-methyl-benzene

生成物 1

HCID 68703601HCID 68703601、化合物収率 87%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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+).

後処理

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

出典と根拠

ORDレコード
ord-d0014ce5ce7a4e52938c1bf911422fa0
出典データセット
uspto-grants-2010_03
特許番号
US07678818B2

反応ノート

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