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

HRID 400628노트

반응식

HRID 400628 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f68f8ed635524fa0ad827e9d633783b5
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741897B2

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