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

HRID 2082361ノート

反応式

HRID 2082361 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4eaf375782284608a3d2fc580d48f8a5
出典データセット
uspto-grants-1993_02
特許番号
US05189045

反応ノート

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