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

HRID 345499

反応式

HRID 345499 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:16])[CH2:14][CH3:15])=[CH:5][CH:4]=1.[CH2:17]=O.Cl.[NH:20]1[CH2:24][CH2:23][CH2:22][CH2:21]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:16])[CH:14]([CH3:17])[CH2:15][N:20]2[CH2:24][CH2:23][CH2:22][CH2:21]2)=[CH:5][CH:4]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 212848Pyrrolidine, hydrochloride (1:1)HCID 149942371-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-1-propanone

生成物 1

HCID 140713261-(4-Methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-methyl-3-pyrrolidino-1-propanone収率 83.9%

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-propanone (4.37g), paraformaldehyde (1.80g), pyrrolidine hydrochloride (3.23g), and hydrochloric acid (0.2 ml) in isopropyl alcohol (50 ml) was refluxed for 8 hours. 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 and then filtered. The filtrate was evaporated in vacuo to give 1-(4-methoxy-5,6,7,8-tetrahydro-1-naphthyl)-2-methyl-3-pyrrolidino -1-propanone. (5.06; yield: 83.9%).

後処理

  1. temperaturewas refluxed for 8 hours
  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. filtrationfiltered
  9. customThe filtrate was evaporated in vacuo

出典と根拠

ORDレコード
ord-26c75cddd09e4ce0890f2852628908e7
出典データセット
uspto-grants-1991_10
特許番号
US05057535

関連ノート

読み込み中…