Sodium Iodide → HCID 12783765、化合物

HRID 1979770ノート

反応式

HRID 1979770 の反応式
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH2:13][CH2:14][CH2:15]Cl)[CH:10]=2)[NH:5][C:4](=[O:17])[CH:3]=1.[I-].[Na+].[CH2:20]([CH:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(=O)([O-])O.[Na+]>C(N(CC)CC)C.CN(C)C=O.CC(C)=O>[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH2:13][CH2:14][CH2:15][N:30]3[CH2:31][CH2:32][CH:27]([CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[CH2:28][CH2:29]3)[CH:10]=2)[NH:5][C:4](=[O:17])[CH:3]=1

参加物

8

反応物 4

HCID 5238Sodium IodideHCID 317384-BenzylpiperidineHCID 516892Sodium BicarbonateHCID 12899554HCID 12899554、化合物

生成物 1

HCID 12783765HCID 12783765、化合物収率 82%

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒

反応条件

温度
50 °C

実験手順

2.5 Grams of 4-methyl-6-(3-chloropropoxy)carbostyril, 1.8 g of sodium iodide were mixed with 50 ml of acetone and the mixture was stirred at 50° C. for 1 hour, then 50 ml of dimethylformamide was added and acetone was removed by distillation under a reduced pressure. To the residue thus obtained was added 1.5 g of triethylamine and 1.6 g of 4-benzylpiperidine and the mixture was heated at 70°-80° C. for 7 hours under stirring condition. The reaction mixture was then concentrated under a reduced pressure to dryness and to the residue thus obtained was added 60 ml of a 5%-sodium hydrogencarbonate aqueous solution and stirred to obtain the insoluble matters. The insoluble matters were collected by filtration, washed with water and then recrystallized from methanol to obtain 3.2 g (yield: 82%) of 4-methyl-6-[3-(4-benzyl-1-piperidyl)propoxy]-carbostyril as in the form of yellowish prism-like crystals. Melting point: 177°-178° C.

後処理

  1. customacetone was removed by distillation under a reduced pressure
  2. customTo the residue thus obtained
  3. temperaturethe mixture was heated at 70°-80° C. for 7 hours
  4. stirringunder stirring condition
  5. concentrationThe reaction mixture was then concentrated under a reduced pressure to dryness and to the residue
  6. customthus obtained
  7. stirringstirred
  8. customto obtain the insoluble matters
  9. filtrationThe insoluble matters were collected by filtration
  10. washwashed with water
  11. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-33d37c4bdd1e42c1af5b43130fa3024f
出典データセット
uspto-grants-1984_11
特許番号
US04482560

反応ノート

読み込み中…