Sodium Dithionite → HCID 57747399, 화합물

HRID 386623노트

반응식

HRID 386623 반응식
[O-]S(S([O-])=O)=O.[Na+].[Na+].[Br:9][C:10]1[CH:46]=[C:45]([CH3:47])[C:13]([O:14][C:15]2[C:20]([N+]([O-])=O)=[C:19](/[CH:24]=[CH:25]/[N:26](C)C)[N:18]=[C:17]([N:29]([C:37]3[CH:42]=[CH:41][C:40]([C:43]#[N:44])=[CH:39][CH:38]=3)[C:30](=[O:36])[O:31][C:32]([CH3:35])([CH3:34])[CH3:33])[N:16]=2)=[C:12]([CH3:48])[CH:11]=1>O.C1COCC1>[Br:9][C:10]1[CH:46]=[C:45]([CH3:47])[C:13]([O:14][C:15]2[C:20]3[NH:26][CH:25]=[CH:24][C:19]=3[N:18]=[C:17]([N:29]([C:37]3[CH:42]=[CH:41][C:40]([C:43]#[N:44])=[CH:39][CH:38]=3)[C:30](=[O:36])[O:31][C:32]([CH3:34])([CH3:33])[CH3:35])[N:16]=2)=[C:12]([CH3:48])[CH:11]=1

참가 물질

5

반응물 2

HCID 24489Sodium DithioniteHCID 57747426HCID 57747426, 화합물

생성물 1

HCID 57747399HCID 57747399, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of Na2S2O4 (40.04 g, 230 mmol) in water (100 ml) was added to a solution of (E)-tert-butyl 4-(4-bromo-2,6-dimethylphenoxy)-6-(2-(dimethylamino)vinyl)-5-nitropyrimidin-2-yl(4-cyanophenyl)carbamate (28.0 g, 45.9 mmol) in THF (300 ml). The mixture was stirred at room temperature of 2 days. The reaction mixture was concentrated. The residue was washed with water and extracted with ethyl acetate. The organic layer was concentrated and the product was obtained by crystallization from a mixture of water and methanol (18.15 g (mmol, 74%). 1H NMR (CDCl3, 400 MHz) δ 1.33 (s, 9H), 2.05 (s, 6H), 6.73 (d, J=3.8 Hz, 1H), 7.18 (d, J=8.8 Hz, 2H), 7.21 (s, 2H), 7.49 (d, J=8.8, 2H), 7.55 (d, J=3.8 Hz, 1H), 9.09 (s, 1H).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. washThe residue was washed with water
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic layer was concentrated
  5. customthe product was obtained by crystallization from a mixture of water and methanol (18.15 g (mmol, 74%)

출처 및 근거

ORD 기록
ord-076a07e4f5e6423e917301d80739401f
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372852B2

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