Hydrochloric Acid → 4-(1-Hydroxy-4-iodobutyl)-alpha,alpha-dimethylphenylacetic acid

HRID 1080502ノート

反応式

HRID 1080502 の反応式
[I:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:9][CH:8]=1)=[O:6].[BH4-].[Na+].Cl>CO>[OH:6][CH:5]([C:7]1[CH:12]=[CH:11][C:10]([C:13]([CH3:18])([CH3:17])[C:14]([OH:16])=[O:15])=[CH:9][CH:8]=1)[CH2:4][CH2:3][CH2:2][I:1]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 113143824-(4Iodo-1-oxobutyl)-alpha,alpha-dimethylphenylacetic acid

生成物 1

HCID 222227064-(1-Hydroxy-4-iodobutyl)-alpha,alpha-dimethylphenylacetic acid収率 79.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 50 mg of 4-(4-iodo-1-oxobutyl)-α,α-dimethylphenylacetic acid, prepared in accordance with Example 3, in 3 mL of methanol was added 50 mg of NaBH4. The mixture was stirred for 30 minutes, acidified with 2N HCl, and the methanol removed in vacuo. The concentrate was extracted with EtOAc. The organics were dried over Na2SO4, filtered, and concentrated to afford 40 mg of 4-(1-hydroxy-4-iodobutyl)-α,α-dimethylphenylacetic acid.

後処理

  1. customthe methanol removed in vacuo
  2. extractionThe concentrate was extracted with EtOAc
  3. dry with materialThe organics were dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-2458dc47a36a4626b720bd387d85a290
出典データセット
uspto-grants-1996_12
特許番号
US05581011

反応ノート

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