Methanol → HCID 68533538、化合物

HRID 736703ノート

反応式

HRID 736703 の反応式
[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

参加物

6

反応物 3

HCID 887MethanolHCID 3939Lithium HydroxideHCID 68533674HCID 68533674、化合物

生成物 1

HCID 68533538HCID 68533538、化合物収率 95%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-e3d590cd19394831acb99e28ea1048b2
出典データセット
uspto-grants-2009_09
特許番号
US07595406B2

反応ノート

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