Potassium Sodium Tartrate → HCID 21891870, 화합물

HRID 1884073노트

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HRID 1884073 반응식
[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

참가 물질

5

반응물 3

HCID 9357Potassium Sodium TartrateHCID 21225700DiisobutylaluminumhydrideHCID 21891959HCID 21891959, 화합물

생성물 1

HCID 21891870HCID 21891870, 화합물수율 80.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d4c1ec4e3ad4e36bca3fe9806e35dab
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06762301B2

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