Aluminium lithium hydride → 3-(5-Fluoro-2-methoxyphenyl)-3-methylbutan-1-ol

HRID 400628ノート

反応式

HRID 400628 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C[O:8][C:9](=O)[CH2:10][C:11]([C:14]1[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=1[O:21][CH3:22])([CH3:13])[CH3:12]>C1COCC1.C(OCC)C>[F:20][C:18]1[CH:17]=[CH:16][C:15]([O:21][CH3:22])=[C:14]([C:11]([CH3:12])([CH3:13])[CH2:10][CH2:9][OH:8])[CH:19]=1

参加物

5

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 57809938Methyl 3-methyl-3-(2-methoxy-5-fluorophenyl)butanoate

生成物 1

HCID 578097383-(5-Fluoro-2-methoxyphenyl)-3-methylbutan-1-ol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of LAH (1.64 g) in 100 mL of THF stirred under argon was added dropwise over 30 minutes a solution of the above 3-(5-fluoro-2-methoxyphenyl)-3-methylbutyric acid methyl ester in 10 mL of THF (vigorous reaction). The mixture was stirred at room temperature overnight. The reaction was diluted with 200 mL of diethyl ether and quenched by the addition of 3 mL of water (added cautiously) and 3 mL of acetic acid. The mixture was filtered through diatomaceous earth and washed through with diethyl ether. Evaporation of the solvent gave 10.8 g of 3-(5-fluoro-2-methoxyphenyl)-3-methylbutan-1-ol, which was used without additional purification.

後処理

  1. stirringThe mixture was stirred at room temperature overnight
  2. customquenched by the addition of 3 mL of water (
  3. additionadded cautiously) and 3 mL of acetic acid
  4. filtrationThe mixture was filtered through diatomaceous earth
  5. washwashed through with diethyl ether
  6. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-f68f8ed635524fa0ad827e9d633783b5
出典データセット
uspto-grants-2014_06
特許番号
US08741897B2

反応ノート

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