Stannous Chloride → HCID 46944973, 화합물

HRID 2370591노트

반응식

HRID 2370591 반응식
Cl[Sn]Cl.[CH3:4][C:5]1([CH3:45])[N:9]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][S:19][CH2:20][CH2:21][CH2:22][C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25])[C:8](=[O:30])[N:7]([C:31]2[CH:36]=[CH:35][C:34]([N+:37]([O-])=O)=[C:33]([C:40]([F:43])([F:42])[F:41])[CH:32]=2)[C:6]1=[O:44].C([O-])(O)=O.[Na+]>CCOC(C)=O>[NH2:37][C:34]1[CH:35]=[CH:36][C:31]([N:7]2[C:6](=[O:44])[C:5]([CH3:45])([CH3:4])[N:9]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][S:19][CH2:20][CH2:21][CH2:22][C:23]([F:28])([F:29])[C:24]([F:25])([F:26])[F:27])[C:8]2=[O:30])=[CH:32][C:33]=1[C:40]([F:43])([F:42])[F:41]

참가 물질

5

반응물 3

HCID 24479Stannous ChlorideHCID 516892Sodium BicarbonateHCID 46947722HCID 46947722, 화합물

생성물 1

HCID 46944973HCID 46944973, 화합물수율 84%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

SnCl2, 2H2O (3.84 g, 17 mmoles) is added to the compound of Example 1 (1.08 g, 1.7 mmole) dissolved in AcOEt (30 ml). The reaction mixture is heated under reflux until the starting compound disappears (5 h 30) and then cooled down using an ice bath. After dilution with AcOEt (30 ml), the mixture is poured onto a 1M aqueous solution of NaHCO3 (120 ml). The mixture is stirred for a few hours during which time a white precipitate forms. This precipitate is eliminated by filtration on celite. The filtrate is decanted and the organic solution is dried over Na2SO4, filtered and concentrated to dryness under vacuum. The expected compound is obtained in the form of a yellow oil with a yield of 84% (868 mg).

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux until the starting compound
  3. custom(5 h 30)
  4. temperaturecooled down
  5. filtrationThis precipitate is eliminated by filtration on celite
  6. customThe filtrate is decanted
  7. dry with materialthe organic solution is dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated to dryness under vacuum

출처 및 근거

ORD 기록
ord-347556575c6949e7a3bfd32ce3f27429
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710091B2

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