1-Chloroethyl chloroformate → 4,5,6,7-Tetrahydro-1-(2-pyridinyl)-1H-imidazo[4,5-c]pyridine

HRID 2177560노트

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HRID 2177560 반응식
C([N:8]1[CH2:13][CH2:12][C:11]2[N:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[CH:15]=[N:16][C:10]=2[CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O>ClCCCl>[N:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[N:14]1[C:11]2[CH2:12][CH2:13][NH:8][CH2:9][C:10]=2[N:16]=[CH:15]1

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 904091645-Benzyl-1-(pyridin-2-yl)-4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine

생성물 1

HCID 904084924,5,6,7-Tetrahydro-1-(2-pyridinyl)-1H-imidazo[4,5-c]pyridine

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
60 °C

실험 절차

To a solution of 5-benzyl-1-(pyridin-2-yl)-4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine (0.13 g, 0.45 mmol) in DCE (5 mL) was added 1-chloroethyl chloroformate (0.10 mL, 0.90 mmoL). The reaction was allowed to stir for 15 min then heated at reflux for 4 h. The reaction was let cool, concentrated, dissolved in MeOH and heated again at 60° C. for 1 h. The reaction was concentrated and the product was used in the next step without further purification (0.075 g, 83%). MS (ESI): mass calculated for C11H12N4, 200.1. m/z found 201.2 [M+H]+.

후처리

  1. temperaturethen heated
  2. temperatureat reflux for 4 h
  3. temperatureThe reaction was let cool
  4. concentrationconcentrated
  5. dissolutiondissolved in MeOH
  6. concentrationThe reaction was concentrated
  7. customthe product was used in the next step without further purification (0.075 g, 83%)

출처 및 근거

ORD 기록
ord-9729992591a94276a8d2fcc080818b3d
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09066946B2

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