Hydrochloric Acid → 2-Methoxy-N-methyl-alpha-(3-methyl-2-thienyl)benzeneethanamine hydrochloride

HRID 486693노트

반응식

HRID 486693 반응식
[CH:1]([N:3](C)[CH:4]([C:14]1[S:15][CH:16]=[CH:17][C:18]=1[CH3:19])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH3:13])=O.[ClH:21]>CO>[ClH:21].[CH3:13][O:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[CH2:5][CH:4]([C:14]1[S:15][CH:16]=[CH:17][C:18]=1[CH3:19])[NH:3][CH3:1]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 22414408N-Formyl-2-methoxy-N-methyl-alpha-(3-methyl-2-thienyl)benzeneethanamine

생성물 1

HCID 224144592-Methoxy-N-methyl-alpha-(3-methyl-2-thienyl)benzeneethanamine hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of 1.83 g of N-formyl-2-methoxy-N-methyl-α-(3-methyl-2-thienyl)benzeneethanamine, 25 ml of methanol, and 25 ml of 3N hydrochloric acid solution was heated for 3 hr under reflux. Methanol was added to clear the solution. The solution was concentrated, the residue was diluted with water, and extracted with ether. The aqueous phase was basified with 2.5N sodium hydroxide solution and extracted with dichloromethane. The combined organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated. An ether solution of the residue was treated with excess ethereal hydrogen chloride. Recrystallization from acetonitrile gave 0.83 g of product, mp 201°-203.5° C.

후처리

  1. temperatureunder reflux
  2. concentrationThe solution was concentrated
  3. additionthe residue was diluted with water
  4. extractionextracted with ether
  5. extractionextracted with dichloromethane
  6. dry with materialThe combined organic phase was dried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. additionAn ether solution of the residue was treated with excess ethereal hydrogen chloride
  10. customRecrystallization from acetonitrile

출처 및 근거

ORD 기록
ord-31dead035bcb42b9af0321c355bd9169
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292760

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