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Methyl 4-(4-chlorophenyl)-4-oxobutanoate → Methyl 4-(4-chlorophenyl)-4-hydroxybutanoate

HRID 22490
ノート
印刷プレビュー

反応式

HRID 22490 の反応式
[BH4-].[Na+].[Cl:3][C:4]1[CH:17]=[CH:16][C:7]([C:8]([CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])=[O:9])=[CH:6][CH:5]=1>CO>[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([CH:8]([OH:9])[CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 230774Methyl 4-(4-chlorophenyl)-4-oxobutanoateHCID 4311764Sodium borohydride

生成物 1

HCID 10513575Methyl 4-(4-chlorophenyl)-4-hydroxybutanoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium borohydride (1.3 g, 35 mmol) was added portionwise to a stirred solution of methyl 3-(4-chlorobenzoyl)propionate (5.3 g, 23 mmol) in methanol (50 ml) at 0° C. The mixture was allowed to warm up to room temperature, stirred for 4 h and partitioned between 1M aqueous hydrochloric acid (100 ml) and DCM (150 ml). The organic layer was separated and the aqueous layer extracted with DCM 2×100 ml). The combined extracts were dried over anhydrous sodium sulphate, filtered and concentrated to give crude methyl 4-(4-chlorophenyl)-4-hydroxybutanoate which was dissolved in methanol (40 ml). Sodium hydride (80% dispersion in oil: 100 mg, 3 mmol) was added, the mixture stirred for 1 h, and partitioned between aqueous 1M hydrochloric acid (50 ml) and ethyl acetate (100 ml). The organic layer was separated and the aqueous layer extracted with ethyl acetate (100 ml). The combined organics were dried over anhydrous potassium carbonate, filtered and concentrated to give 5-(4-chlorophenyl)-gamma-butyrolactone (3.85 g, 83%) as a colourless oil.

後処理

  1. custompartitioned between 1M aqueous hydrochloric acid (100 ml) and DCM (150 ml)
  2. customThe organic layer was separated
  3. extractionthe aqueous layer extracted with DCM 2×100 ml)
  4. dry with materialThe combined extracts were dried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-a19cc6165bfe4e058501fafc67b19680
出典データセット
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05428168

反応ノート

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