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Ammonium Chloride → HCID 68521214, 화합물

HRID 522852
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HRID 522852 반응식
[CH:1]1([C:4]2[CH:5]=[C:6]3[C:11](=[CH:12][CH:13]=2)[CH:10]=[N:9][CH:8]=[CH:7]3)[CH2:3][CH2:2]1.[In].[NH4+].[Cl-]>CCO>[CH:1]1([C:4]2[CH:5]=[C:6]3[C:11](=[CH:12][CH:13]=2)[CH2:10][NH:9][CH2:8][CH2:7]3)[CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 5359967IndiumHCID 67355115HCID 67355115, 화합물

생성물 1

HCID 68521214HCID 68521214, 화합물수율 58%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 6-cyclopropylisoquinoline (0.500 g, 0.003 mol) in EtOH (15 mL) was added indium powder (3 g) and saturated aqueous NH4Cl (5 mL). The reaction mixture was heated at reflux for 36 h while stirring. After completion, the reaction mixture was filtered through Celite® (diatomaceous earth) and the filtrate concentrated at reduced pressure to afford crude 6-cyclopropyl-1,2,3,4-tetrahydro-isoquinoline. Purification was done by silica gel column chromatography eluting with MeOH in CH2Cl2 (0-10%) to afford pure 6-cyclopropyl-1,2,3,4-tetrahydro-isoquinoline (0.300 g, 58%) as a white solid.

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후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 36 h
  3. filtrationAfter completion, the reaction mixture was filtered through Celite® (diatomaceous earth)
  4. concentrationthe filtrate concentrated at reduced pressure
  5. customto afford crude 6-cyclopropyl-1,2,3,4-tetrahydro-isoquinoline
  6. customPurification
  7. washeluting with MeOH in CH2Cl2 (0-10%)

출처 및 근거

ORD 기록
ord-fdf43fb32a1241deb4c5580d4a57d6d9
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09334269B2

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