Sodium hydride → HCID 10764229, 화합물

HRID 1069606

반응식

HRID 1069606 반응식
[CH2:1]([O:3][C:4](=[O:18])[CH2:5][C:6]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH3:16])[CH:13]=2)[NH:8][C:7]=1[CH3:17])[CH3:2].[H-].[Na+].Br[CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O>[CH2:1]([O:3][C:4](=[O:18])[CH2:5][C:6]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:15][CH3:16])[CH:13]=2)[N:8]([CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:7]=1[CH3:17])[CH3:2]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2633651-(Bromomethyl)-2-phenylbenzeneHCID 10729163Ethyl (5-methoxy-2-methyl-1H-indol-3-yl)acetate

생성물 1

HCID 10764229HCID 10764229, 화합물수율 72%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1-([1,11′-Biphenyl]-2-ylmethyl)-5-methoxy,y-2-methyl-1H-indole-3-acetic acid ethyl ester. 5-Methoxy-2-methyl-1H-indole-3-acetic acid ethyl ester (988 mg, 4 mmol) was added to 160 mg (4 mmol) of NaH/mineral oil (previously washed with hexane), the mixture stirred for 0.5 hours and 0.74 mL (4 mmol) of2- (bromomethyl) biphenyl added. After 2 hours, water was added and the mixture extracted with ethyl acetate. The ethyl acetate was washed with brine, dried (MgSO4) and concentrated at reduced pressure. The residue was chromatographed on silica gel eluting with 20% EtOAc/hexane to give 1.18 g (72% yield) of 1-([1,1′-biphenyl]-2-ylmethyl)-5-methoxy-2-methyl-1H-indole-3-acetic acid ethyl ester as an oil.

후처리

  1. washpreviously washed with hexane), the mixture
  2. waitAfter 2 hours
  3. extractionthe mixture extracted with ethyl acetate
  4. washThe ethyl acetate was washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated at reduced pressure
  7. customThe residue was chromatographed on silica gel eluting with 20% EtOAc/hexane

출처 및 근거

ORD 기록
ord-7116ac58940b4af186b494fa8da01608
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06252084B1

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