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1,2-Dimethoxyethane → HCID 12392200, 화합물

HRID 1973400
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HRID 1973400 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].COCCOC.[NH:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:15]([C:22](=O)[C:23]([N:25]2[CH2:30][CH2:29][N:28]([N:31]=O)[CH2:27][CH2:26]2)=O)=[CH:14]1>O>[NH2:31][N:28]1[CH2:29][CH2:30][N:25]([CH2:23][CH2:22][C:15]2[C:16]3[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=3)[NH:13][CH:14]=2)[CH2:26][CH2:27]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80711,2-Dimethoxyethane2회HCID 12392195HCID 12392195, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 12392200HCID 12392200, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
-5 °C

실험 절차

To a stirred mixture of 9.0 g of lithium aluminum hydride in 400 ml. of 1,2-dimethoxyethane is added 10.52 g (0.037 mol) of 1-(indol-3-ylglyoxyloyl)-4-nitrosopiperazine slowly to maintain reaction temperature below 35° C. After all the material is added, the mixture is refluxed for 14-16 hours. The reaction mixture is cooled to -5° C. and a solution of 50 ml. of water and 50 ml. of 1,2-dimethoxyethane is slowly added while maintaining the temperature below 15° C. Another 50 ml. of water is added, and the mixture is then filtered. The solvent is removed from the filtrate and the residual solid is recrystallized from benzene, producing the pure crystals of 3-[2-(4-aminopiperazin-1-yl)ethyl]indole, m.p. 115°-117° C. Analysis: Calculated for C14H20N4 :68.82% C; 8.25% H; 22.93% N Found:68.70% C; 8.17% H; 22.55% N.

후처리

  1. temperatureto maintain
  2. customreaction temperature below 35° C
  3. additionAfter all the material is added
  4. temperaturethe mixture is refluxed for 14-16 hours
  5. temperaturewhile maintaining the temperature below 15° C
  6. filtrationthe mixture is then filtered
  7. customThe solvent is removed from the filtrate
  8. customthe residual solid is recrystallized from benzene

출처 및 근거

ORD 기록
ord-c5c7f99f8f394e7eb935d5fdfe19a1d1
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03997539

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