Sodium Sulfate → (1-Methyl-1H-indol-6-yl)methanol

HRID 1058361노트

반응식

HRID 1058361 반응식
C[O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([CH:9]=[CH:10][N:11]2[CH3:14])=[CH:7][CH:6]=1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].[O-]S([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[CH3:14][N:11]1[C:12]2[C:8](=[CH:7][CH:6]=[C:5]([CH2:3][OH:2])[CH:13]=2)[CH:9]=[CH:10]1

참가 물질

5

반응물 3

HCID 24436Sodium SulfateHCID 639843Methyl N-methylindole-6-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 18673032(1-Methyl-1H-indol-6-yl)methanol수율 79.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of 1-methyl-1H-indole-6-carboxylic acid methyl ester (Example 15; 2.52 g, 13.3 mmol) in diethyl ether (50 mL) was added to a suspension of lithium aluminum hydride (0.50 g, 13.2 mmol) in diethyl ether (50 mL) and the mixture was stirred at room temperature for 5 h. Saturated Na2SO4 solution was added (˜5 mL) and the mixture was stirred at room temperature for 30 min, then filtered and the filtrate was dried (MgSO4), overnight. The mixture was filtered and evaporated to furnish 1-methyl-1H-indole-6-methanol (1.70 g, 79% yield) as a colorless oil that solidified on standing, mp 47-49° C.

후처리

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. filtrationfiltered
  3. dry with materialthe filtrate was dried (MgSO4), overnight
  4. filtrationThe mixture was filtered
  5. customevaporated

출처 및 근거

ORD 기록
ord-98549dc4656e44e58b273e790cfdedd8
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06515124B2

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