Hydrochloric Acid → N-{1-[(2,3-dihydrobenzofuran-2-yl)-methyl]-piperid-4-yl}-N-methylpropionamide hydrochloride

HRID 2082361노트

반응식

HRID 2082361 반응식
C(O)(=O)C.[NH:5]1[CH2:10][CH2:9][CH:8]([N:11]([CH3:16])[C:12](=[O:15])[CH2:13][CH3:14])[CH2:7][CH2:6]1.CN(C)C=O.I[CH2:23][CH:24]1[CH2:28][C:27]2[CH:29]=[CH:30][CH:31]=[CH:32][C:26]=2[O:25]1.[ClH:33]>C(N(CC)CC)C>[ClH:33].[O:25]1[C:26]2[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=2[CH2:28][CH:24]1[CH2:23][N:5]1[CH2:10][CH2:9][CH:8]([N:11]([CH3:16])[C:12](=[O:15])[CH2:13][CH3:14])[CH2:7][CH2:6]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 3255132-(Iodomethyl)-2,3-dihydro-1-benzofuranHCID 67858297N-piperid-4-yl-N-methylpropionamide acetate

생성물 1

HCID 19761298N-{1-[(2,3-dihydrobenzofuran-2-yl)-methyl]-piperid-4-yl}-N-methylpropionamide hydrochloride수율 30%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

5.1 g of N-piperid-4-yl-N-methylpropionamide acetate, 90 ml of dimethylformamide and 6.3 ml of triethylamine are introduced into a 250 ml three-necked flask. 6.6 g of 2,3-dihydro-2-iodomethylbenzofuran are poured onto the mixture which is heated to 60°-65° C. This temperature is maintained for 15 hours. The reaction mixture is evaporated to dryness and the residue is taken up in ethyl acetate and extracted with 150 ml of N hydrochloric acid. The aqueous phase is rendered alkaline with sodium hydroxide in the presence of ethyl acetate. The organic phase is washed with water and dried over magnesium sulphate. The solvent is evaporated to yield a base in the form of a brown oil, which is converted into a salt with 3.8N ethereal hydrogen chloride to yield the desired compound.

후처리

  1. temperatureis heated to 60°-65° C
  2. temperatureThis temperature is maintained for 15 hours
  3. customThe reaction mixture is evaporated to dryness
  4. extractionextracted with 150 ml of N hydrochloric acid
  5. washThe organic phase is washed with water
  6. dry with materialdried over magnesium sulphate
  7. customThe solvent is evaporated
  8. customto yield a base in the form of a brown oil, which

출처 및 근거

ORD 기록
ord-4eaf375782284608a3d2fc580d48f8a5
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05189045

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