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Acetone → HCID 67177037, 화합물

HRID 1966008
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HRID 1966008 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:13][CH2:12][CH2:11][NH:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.[CH2:15]=O.O.[CH3:18][C:19]([CH3:21])=[O:20]>C(O)(C)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:13][CH2:12][CH2:11][N:10]2[CH2:15][CH2:18][C:19](=[O:20])[CH3:21])[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 180Acetone2회HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 962WaterHCID 34467312-(3,4-dichlorophenyl)pyrrolidine

생성물 1

HCID 67177037HCID 67177037, 화합물

시약·촉매·용매 1

HCID 3776
Isopropanol
용매

실험 절차

To the solution of 4 g (18.5 mmol) 2-(3,4-dichlorophenyl)-pyrrolidine in 10 ml acetone, during ice-water cooling, the mixture of 10 ml acetone and 1.6 ml cc. hydrochloric acid is added. The mixture is stirred for 15 minutes under cooling for 10 minutes at room temperature, then the solution of 0.83 g (9.3 mmol) paraformaldehyde in 9.2 ml iso-propanol is added and the reaction mixture is heated at reflux temperature for 4 hours. After cooling, 15 ml of water is added and the mixture is extracted with 3×20 ml dichloromethane, dried over sodium sulfate and evaporated in vacuum. The residue is crystallized in hexane to obtain 2.11 g title compound. Mp: 160-162° C.

후처리

  1. temperaturethe reaction mixture is heated
  2. temperatureat reflux temperature for 4 hours
  3. temperatureAfter cooling
  4. extractionthe mixture is extracted with 3×20 ml dichloromethane
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuum
  7. customThe residue is crystallized in hexane

출처 및 근거

ORD 기록
ord-bf23fe56ee164ce295a328208b527835
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420636B2

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