2-Methyl-6-phenoxy-hexanoic acid → 1-Hydroxy-2-methyl-6-phenoxyhexane

HRID 1287353노트

반응식

HRID 1287353 반응식
[CH3:1][CH:2]([CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:3](O)=[O:4].[H-].[H-].[H-].[H-].[Li+].[Al+3]>CCOCC.C1COCC1>[OH:4][CH2:3][CH:2]([CH3:1])[CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

5

반응물 2

HCID 203221352-Methyl-6-phenoxy-hexanoic acidHCID 21226445Aluminium lithium hydride2회

생성물 1

HCID 203221341-Hydroxy-2-methyl-6-phenoxyhexane

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 129 g of 2-methyl-6-phenoxy-hexanoic acid in 200 ml of absolute ether and 100 ml of absolute THF was added dropwise, under exclusion of humidity, to 32 g (0.84 mol) of LiAlH4 in 1.2 l of absolute ether. After reflux and stirring for 5 hours the LiAlH4 in excess was destroyed with acetic acid and then destroyed by dropwise addition of water and a 10% sulfuric acid. The organic layer was washed with saturated NaHCO3 -solution, dried and evaporated. The crude product was immediately further reacted.

후처리

  1. temperatureAfter reflux
  2. customin excess was destroyed with acetic acid
  3. customdestroyed by dropwise addition of water
  4. washThe organic layer was washed with saturated NaHCO3 -solution
  5. customdried
  6. customevaporated

출처 및 근거

ORD 기록
ord-24f4068b27994f578d97f3b06877d331
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03984459

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