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Hydrogen Bromide → 1-[1-(4-Chlorophenyl)cyclobutyl]-2-ethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrobromide

HRID 440489
ノート
印刷プレビュー

反応式

HRID 440489 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH:12]3[C:21]4[C:16](=[CH:17][C:18]([O:24]C)=[C:19]([O:22]C)[CH:20]=4)[CH2:15][CH2:14][NH:13]3)[CH2:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[CH2:26](I)[CH3:27].C(=O)([O-])[O-].[K+].[K+].[BrH:35]>C(O)(=O)C.C(N(CC)CC)C.CC(C)=O>[BrH:35].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([CH:12]3[C:21]4[C:16](=[CH:17][C:18]([OH:24])=[C:19]([OH:22])[CH:20]=4)[CH2:15][CH2:14][N:13]3[CH2:26][CH3:27])[CH2:9][CH2:10][CH2:11]2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 260Hydrogen BromideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 224067941-[1-(4-Chlorophenyl)cyclobutyl]-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 224067431-[1-(4-Chlorophenyl)cyclobutyl]-2-ethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrobromide

試薬・触媒・溶媒 3

HCID 176
Acetic Acid
溶媒
HCID 180Acetone溶媒
HCID 8471Triethylamine溶媒

実験手順

A mixture of 1-[1-(4-chlorophenyl)cyclobutyl]-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline (7.29 g prepared as described in Example 50), ethyl iodide (1.76 ml), anhydrous potassium carbonate (5.52 g) and acetone (100 ml) was heated under reflux for 16 hours. The reaction mixture was filtered and the solvent was removed by evaporation to give a residue which was digested with a 9:1 mixture of petroleum ether and triethylamine. The solution was filtered and the solvent removed to give a residue. A sample of this residue (4 g) was heated under reflux in a nitrogen atmosphere with glacial acetic acid (40 ml) and 48% hydrobromic acid (40 ml) for 20 hours. Removal of the solvent gave a residue which was dried by azeotropic distillation with industrial methylated spirit, then with propan-2-ol and finally with a mixture of toluene and propan-2-ol to give a solid which was washed with propan-2-ol and dried in vacuo at 80° C. to give 1-[1-(4-chlorophenyl)cyclobutyl]-2-ethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrobromide, m.p. 213°-215° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. filtrationThe reaction mixture was filtered
  4. customthe solvent was removed by evaporation
  5. customto give a residue which
  6. filtrationThe solution was filtered
  7. customthe solvent removed
  8. customto give a residue
  9. customRemoval of the solvent
  10. customgave a residue which
  11. dry with materialwas dried by azeotropic distillation with industrial methylated spirit
  12. additionwith propan-2-ol and finally with a mixture of toluene and propan-2-ol
  13. customto give a solid which
  14. washwas washed with propan-2-ol
  15. customdried in vacuo at 80° C.

出典と根拠

ORDレコード
ord-bd0e793d69b3407b82a85093061a52cc
出典データセット
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05519034

反応ノート

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