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Water → 2-Hydroxymethyl-8-methoxy-chroman

HRID 1728322
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반응식

HRID 1728322 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[O:11][CH:10]([C:13](OCC)=[O:14])[CH2:9][CH2:8]2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1.C(OCC)C>[OH:14][CH2:13][CH:10]1[CH2:9][CH2:8][C:7]2[C:12](=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][CH:6]=2)[O:11]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 18787171Ethyl 8-methoxy-chroman-2-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 234318182-Hydroxymethyl-8-methoxy-chroman

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

59.0 g (0.25 mol) of ethyl 8-methoxy-chroman-2-carboxylate in 525 ml of anhydrous tetrahydrofuran are added dropwise to a suspension of 9.5 g (0.25 mol) of lithium aluminium hydride in 525 ml of anhydrous diethyl ether at 20° C. in the course of 1 hour, while stirring. The mixture is stirred overnight, and 9.5 ml of water, 9.5 ml of 15% strength sodium hydroxide solution and 28.4 ml of water are then added dropwise in succession, while cooling. The organic phase is decanted and evaporated. The residue is recrystallised twice from methylene chloride/petroleum ether.

후처리

  1. stirringThe mixture is stirred overnight
  2. temperaturewhile cooling
  3. customThe organic phase is decanted
  4. customevaporated
  5. customThe residue is recrystallised twice from methylene chloride/petroleum ether

출처 및 근거

ORD 기록
ord-b32a360a7e074eb192b6ab0a14ec39a5
출처 데이터셋
uspto-grants-1994_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05326771

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