Hydrochloric Acid → 1-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1)

HRID 12490

반응식

HRID 12490 반응식
[ClH:1].[C:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)(=[O:4])[CH3:3].[CH2:11]=O.Cl.[CH3:14][NH:15][CH3:16]>CCO>[ClH:1].[CH3:14][N:15]([CH3:11])[CH2:16][CH2:3][C:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 7410AcetophenoneHCID 10473Dimethylamine, hydrochloride

생성물 1

HCID 928441-Propanone, 3-(dimethylamino)-1-phenyl-, hydrochloride (1:1)

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 0.5 mL concentrated aqueous HCl in 40 mL EtOH, acetophenone (30.0 g), paraformaldehyde (10.0 g) and dimethylamine hydrochloride (26.5 g) were added and the mixture was refluxed for 3 h. The mixture was cooled to room temperature, and the precipitate was filtered, washed with acetone and dried in vacuo to obtain 37.2 g of white crystalline material. 1H NMR (200 MHz, DMSO-d6) δ 2.84 (s, 6H), 3.38-3.55 (m, 2H), 3.57-3.74 (m, 2H), 7.48-7.73 (m, 3H), 7.97-8.10 (m, 2H).

후처리

  1. temperaturethe mixture was refluxed for 3 h
  2. filtrationthe precipitate was filtered
  3. washwashed with acetone
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-82bf5f4e932d4b81942421c22a32c6e8
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728018B2

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