Potassium Sodium Tartrate → HCID 21891870、化合物

HRID 720502ノート

反応式

HRID 720502 の反応式
[Cl:1][C:2]1[C:11]([C:12](OCC)=[O:13])=[C:10]([CH2:17][N:18]2[CH2:23][CH2:22][N:21]([CH3:24])[CH2:20][CH2:19]2)[C:9]2[C:4](=[CH:5][C:6]([Cl:27])=[C:7]([O:25][CH3:26])[CH:8]=2)[N:3]=1.[H-].C([Al+]CC(C)C)C(C)C.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C(Cl)Cl>[Cl:1][C:2]1[C:11]([CH2:12][OH:13])=[C:10]([CH2:17][N:18]2[CH2:19][CH2:20][N:21]([CH3:24])[CH2:22][CH2:23]2)[C:9]2[C:4](=[CH:5][C:6]([Cl:27])=[C:7]([O:25][CH3:26])[CH:8]=2)[N:3]=1

参加物

5

反応物 3

HCID 9357Potassium Sodium TartrateHCID 21225700DiisobutylaluminumhydrideHCID 21891959HCID 21891959、化合物

生成物 1

HCID 21891870HCID 21891870、化合物収率 80.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

ethyl 2,7-dichloro-6-methoxy-4-[(4-methyl-1-piperazinyl)methyl]-3-quinolinecarboxylate (6 g, 14.5 mmol) is dissolved in methylene chloride (120 ml). A molar solution of diisobutylaluminium hydride in methylene chloride (60 ml, 60 mmol) is added slowly. Agitation is carried out for one hour at ambient temperature. The reaction mass is slowly poured into 300 ml of a 20% solution of Rochelle salt. Agitation is carried out for one hour, followed by filtering on celite and decanting; the organic phase is washed with a saturated solution of sodium chloride, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The solid is taken up in isopropyl ether, filtered and dried under vacuum. 4.3 g of sought product (80%) is obtained, in the form of a yellow solid.

後処理

  1. waitAgitation is carried out for one hour
  2. filtrationby filtering on celite
  3. customdecanting
  4. washthe organic phase is washed with a saturated solution of sodium chloride
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. filtrationfiltered
  9. customdried under vacuum

出典と根拠

ORDレコード
ord-5bc69d85767141ceb636a9e684340520
出典データセット
uspto-grants-2006_11
特許番号
US07135478B2

反応ノート

読み込み中…