Hydrochloric Acid → 1-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone

HRID 345497

反応式

HRID 345497 の反応式
[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13](=[O:17])[CH2:14][CH2:15][CH3:16])=[CH:5][CH:4]=1.[CH2:18]=O.Cl.[NH:21]1[CH2:25][CH2:24][CH2:23][CH2:22]1.Cl>C(O)(C)C>[CH3:1][O:2][C:3]1[C:12]2[CH2:11][CH2:10][CH2:9][CH2:8][C:7]=2[C:6]([C:13](=[O:17])[CH:14]([CH2:15][CH3:16])[CH2:18][N:21]2[CH2:25][CH2:24][CH2:23][CH2:22]2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 212848Pyrrolidine, hydrochloride (1:1)HCID 149942361-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-1-butanone

生成物 1

HCID 140713341-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone収率 62.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 1-(4-methoxy-5,6,7,8-tetrahydro-1-naphthyl)-1-butanone (2.50g), paraformaldehyde (0.42g), pyrrolidine hydrochloride (1.51g), and hydrochloric acid (0.2 ml) in isopropyl alcohol (7 ml) was refluxed for 15 hrs. The reaction mixture was evaporated in vacuo to give the residue. The residue was partitioned into water and ethyl ether. The aqueous layer, was extracted, neutralized with ammonia water, and then extracted with ethyl ether. The organic layer was dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrate was evaporated in vacuo to give 1-(4-methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-ethyl-3-pyrrolidino-1-propanone (2.13 g, Yield: 62.8 %) as an oil.

後処理

  1. temperaturewas refluxed for 15 hrs
  2. customThe reaction mixture was evaporated in vacuo
  3. customto give the residue
  4. customThe residue was partitioned into water and ethyl ether
  5. extractionThe aqueous layer, was extracted
  6. extractionextracted with ethyl ether
  7. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  8. filtrationThe mixture was filtered
  9. customthe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-c8f0fe61614e40adb00ef055c2d4b977
出典データセット
uspto-grants-1991_10
特許番号
US05057535

関連ノート

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