Methanol → HCID 68533538, 화합물

HRID 736703노트

반응식

HRID 736703 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13]C)=[O:12])=[C:9]([F:17])[CH:8]=1.[OH-].[Li+].CO>O1CCCC1.O>[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:16]=[CH:15][C:10]([C:11]([OH:13])=[O:12])=[C:9]([F:17])[CH:8]=1

참가 물질

6

반응물 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68533674HCID 68533674, 화합물

생성물 1

HCID 68533538HCID 68533538, 화합물수율 95%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of EXAMPLE 22A (1.9 g) in tetrahydrofuran (10 mL) and water (5 mL) was added lithium hydroxide (1 g) in water (5 mL). Methanol was added until homogeneous and the solution stirred at ambient temperature for 4 hours. The mixture was concentrated to 5 mL and the residue acidified to pH 2 with 2 N hydrochloric acid. Ethyl acetate and water were added and the organic phase separated, washed with water, dried over magnesium sulfate, filtered and concentrated to give the title compound (1.7 g, 95%). MS (DCI): m/z 227 (M+H)+.

후처리

  1. concentrationThe mixture was concentrated to 5 mL
  2. additionEthyl acetate and water were added
  3. customthe organic phase separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e3d590cd19394831acb99e28ea1048b2
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07595406B2

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