Potassium Carbonate → HCID 10361909、化合物

HRID 1451632ノート

反応式

HRID 1451632 の反応式
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1.Cl.[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][NH:23][CH2:22][CH2:21]2.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:16][O:17][C:18]1[CH:19]=[C:20]2[C:25](=[CH:26][C:27]=1[O:28][CH3:29])[CH2:24][N:23]([CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][CH:7]=1)[CH2:22][CH2:21]2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2611281-(3-Bromopropoxy)-4-nitrobenzeneHCID 64560356,7-Dimethoxy-1,2,3,4-tetrahydroisoquinoline hydrochloride

生成物 1

HCID 10361909HCID 10361909、化合物収率 79.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-(3-bromopropoxy)-4-nitrobenzene (10 g), 1,2,3,4-tetrahydro-6,7-dimethoxyisoquinoline hydrochloride (8.8 g) and potassium carbonate (10.6 g) in DMF (100 ml) was heated at 100° for 16 h. The mixture was then filtered and the filtrate evaporated. The residue was taken up in water and extracted with dichloromethane. The organic layer was washed with water, dried, and evaporated to give an oil which crystallised in ether to give the title compound (11.3 g), m.p. 100°.

後処理

  1. temperaturewas heated at 100° for 16 h
  2. filtrationThe mixture was then filtered
  3. customthe filtrate evaporated
  4. extractionextracted with dichloromethane
  5. washThe organic layer was washed with water
  6. customdried
  7. customevaporated
  8. customto give an oil which
  9. customcrystallised in ether

出典と根拠

ORDレコード
ord-ca46219a13b54da39dd6280e340590a1
出典データセット
uspto-grants-1997_02
特許番号
US05604237

反応ノート

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