Water → HCID 12598593, 화합물

HRID 1071615노트

반응식

HRID 1071615 반응식
[CH3:1][CH:2]([CH3:10])[CH2:3][CH2:4][C:5]([O:7]CC)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O1[CH2:21][CH2:20][CH2:19][CH2:18]1.O.[OH-].[Na+].O1CC[CH2:27][CH2:26]1>C(OCC)C>[CH3:10][CH:2]([CH3:1])[CH:3]([C:18]1[CH:27]=[CH:26][CH:21]=[CH:20][CH:19]=1)[CH2:4][CH2:5][OH:7]

참가 물질

7

반응물 5

HCID 962Water2회HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 117477Ethyl 4-methylpentanoateHCID 68718528lithium aluminium hydride THF

생성물 1

HCID 12598593HCID 12598593, 화합물수율 42%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Under a nitrogen atmosphere, ethyl 4-methylpentanoate (350 mg) was dissolved in tetrahydrofuran (10 mL) at −78° C., a lithium aluminum hydride/tetrahydrofuran solution (1.0 M, 1.58 mL) was added, and the mixture was stirred. While the temperature of the mixture was naturally returned to room temperature, the mixture was stirred, and after 1.5 hours, water (0.05 mL), a 2N aqueous sodium hydroxide (0.05 mL) and water (0.15 mL) were successively added thereto, and the mixture was stirred. Further, diethyl ether was added thereto, and then the resulting insoluble matters were filtered off and the filtrate was evaporated. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate system), to give the title compound as a colorless oil (257 mg, 42%: 2 steps).

후처리

  1. customwas naturally returned to room temperature
  2. stirringthe mixture was stirred
  3. stirringthe mixture was stirred
  4. filtrationthe resulting insoluble matters were filtered off
  5. customthe filtrate was evaporated
  6. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate system)

출처 및 근거

ORD 기록
ord-cb47566cf49245fb83e68747abce4840
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06906072B1

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