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Sodium hydride → HCID 20399406, 화합물

HRID 1981355
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HRID 1981355 반응식
[CH3:1][C:2]1[N:3]([CH2:8][CH2:9][CH2:10][OH:11])[C:4]([CH3:7])=[CH:5][CH:6]=1.[H-].[Na+].Cl[C:15]1[CH:20]=[C:19]([C:21]([N:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)=[O:22])[CH:18]=[CH:17][N:16]=1>COCCOC>[CH3:1][C:2]1[N:3]([CH2:8][CH2:9][CH2:10][O:11][C:17]2[CH:18]=[C:19]([C:21]([N:23]3[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]3)=[O:22])[CH:20]=[CH:15][N:16]=2)[C:4]([CH3:7])=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 128941182,5-Dimethyl-1H-pyrrole-1-propanolHCID 18771703(2-Chloropyridin-4-yl)(piperidin-1-yl)methanone

생성물 1

HCID 20399406HCID 20399406, 화합물수율 102.5%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To a suspension of 0.047 mol of 2.5-dimethyl-1-(3-hydroxypropyl)pyrrole and 0.059 mol of 80% sodium hydride in 150 ml of 1,2-dimethoxyethane, previously heated at reflux for 15 minutes and cooled, is added 0.044 mol of 2-chloro-4-piperidino carbonylpyridine, then the reaction mixture is heated two hours with reflux and evaporated to dryness. The residue is taken up with water and extracted with ethyl acetate. The organic phase is separated and evaporated to dryness. Thus, 15.4 g of an oily product are obtained.

후처리

  1. temperaturepreviously heated
  2. temperatureat reflux for 15 minutes
  3. temperaturecooled
  4. temperaturethe reaction mixture is heated two hours
  5. temperaturewith reflux
  6. customevaporated to dryness
  7. extractionextracted with ethyl acetate
  8. customThe organic phase is separated
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-fff140c4919a4331b0708ce900434650
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04514408

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