Water → 2-(2,3-dihydro-1H-inden-2-yl)ethanol

HRID 1289439노트

반응식

HRID 1289439 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:9][CH:8]1[CH2:16][C:17](OC)=[O:18].O.[OH-].[Na+]>O1CCCC1>[CH2:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:7][CH:8]1[CH2:16][CH2:17][OH:18]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 14090225Methyl (2,3-dihydro-1H-inden-2-yl)acetateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 103520002-(2,3-dihydro-1H-inden-2-yl)ethanol수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Suspended in 100 ml of tetrahydrofuran were 1.02 g (26.8 mmol) of lithium aluminum hydride, and a solution of 5.06 g (26.6 mmol) of methyl (indan-2-yl)acetate in 10 ml of tetrahydrofuran was added dropwise to the suspension while chilling with ice water. After the addition, the mixture was stirred for 1 hour, and 1 ml of water, 1 ml of 15% sodium hydroxide and 3 ml of water were successively added dropwise to the mixture to decompose excess of the reducing agent. Solids were separated by filtration, the filtrate was concentrated, and the residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4), thereby obtaining 4.30 g of a colorless oily substance. Yield: 100%.

후처리

  1. additionAfter the addition
  2. customSolids were separated by filtration
  3. concentrationthe filtrate was concentrated
  4. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4)
  5. customobtaining 4.30 g of a colorless oily substance

출처 및 근거

ORD 기록
ord-915dc59cc4114cc29cb2349948bb1c29
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05750524

반응 노트

불러오는 중…