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Trimethyl orthoformate → 7-Ethyl-alpha-(phenylmethyl)-1H-indole-3-acetic Acid Methyl Ester

HRID 652367
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HRID 652367 반응식
[CH2:1]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:11]=1[NH:10][CH:9]=[C:8]2[CH2:12][C:13](=O)[CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17]C=1)[CH3:2].[CH3:22][O:23][CH:24](OC)[O:25]C.O.O.O.[N+]([O-])([O-])=O.[Tl+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[Tl+]>CCOCC.CO>[CH3:22][O:23][C:24](=[O:25])[CH:12]([CH2:13][C:14]1[CH:15]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:8]1[C:7]2[C:11](=[C:3]([CH2:1][CH3:2])[CH:4]=[CH:5][CH:6]=2)[NH:10][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 9005Trimethyl orthoformateHCID 24937Thallous nitrateHCID 11270721Nitric acid,thallium(3+) salt, trihydrate (9CI)HCID 569785881-(7-ethyl-1H-indol-3-yl)-3-phenylpropanone

생성물 1

HCID 142014387-Ethyl-alpha-(phenylmethyl)-1H-indole-3-acetic Acid Methyl Ester

시약·촉매·용매 2

HCID 887
Methanol
용매
HCID 3283Diethyl Ether용매

실험 절차

According to the procedure of E. C. Taylor et al, J. Amer. Chem. Soc., 98, 3037 (1976), a solution of 1-(7-ethyl-1H-indol-3-yl)-3-phenylpropanone (2.77 g, 10 mmol) in a 1:1 mixture of methanol and trimethylorthoformate (25 mL) was added to thallium (III) nitrate trihydrate (4.88 g, 11 mmol), and the mixture was heated under reflux until precipitation of thallium (I) nitrate was complete (about 3 hours). The dark brown mixture was diluted with 25 mL of ether, and the thallium (I) nitrate was removed by filtration. The filtrate was washed successively with 1×50 mL portions of water, 5% aqueous sodium bicarbonate, and water and was then dried over anhydrous MgSO4. Concentration of the filtrate and flash chromatography of the crude product (20% ethyl acetate/hexane, silica gel) have the ester as a red-brown oil (0.98 g, 31.9%).

후처리

  1. temperaturethe mixture was heated
  2. custom(about 3 hours)
  3. customthe thallium (I) nitrate was removed by filtration
  4. washThe filtrate was washed successively with 1×50 mL portions of water, 5% aqueous sodium bicarbonate, and water
  5. dry with materialwas then dried over anhydrous MgSO4

출처 및 근거

ORD 기록
ord-9f7d841405854dca903f6b9cae27acd1
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04670462

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