2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 58392263, 화합물

HRID 561380

반응식

HRID 561380 반응식
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[C:4]([F:10])[CH:3]=1.[CH3:11][C:12]1([CH3:20])[O:19][C:17](=[O:18])[CH2:16][C:14](=[O:15])[O:13]1.[F:21][C:22]1[CH:23]=[C:24]2[C:28](=[C:29]([CH2:31][S:32][CH3:33])[CH:30]=1)[NH:27][CH:26]=[CH:25]2>C(#N)C.N1CCCC1C(O)=O>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]([C:25]2[C:24]3[C:28](=[C:29]([CH2:31][S:32][CH3:33])[CH:30]=[C:22]([F:21])[CH:23]=3)[NH:27][CH:26]=2)[CH:16]2[C:17](=[O:18])[O:19][C:12]([CH3:20])([CH3:11])[O:13][C:14]2=[O:15])=[C:4]([F:10])[CH:3]=1

참가 물질

6

반응물 3

HCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 27249084-Chloro-2-fluorobenzaldehydeHCID 583922275-Fluoro-7-[(methylsulfanyl)methyl]-1H-indole

생성물 1

HCID 58392263HCID 58392263, 화합물수율 103.9%

시약·촉매·용매 2

HCID 614proline dl-form촉매HCID 6342Acetonitrile용매

실험 절차

0.70 g (4.41 mmol) of 4-chloro-2-fluorobenzaldehyde, 0.64 g (4.41 mmol) of Meldrum's acid and 24 mg (0.21 mmol) of D,L-proline were added to a solution of 1.00 g of the compound of Example 11A with a purity of 82% (4.20 mmol) in 35 ml of acetonitrile. The reaction mixture was stirred at RT overnight. It was concentrated, and the residue was taken up in ethyl acetate, washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution and water, dried over magnesium sulfate, filtered and concentrated. 2.20 g of the title compound were obtained with a purity of 71% (78% of theory) and were reacted without further purification.

후처리

  1. concentrationIt was concentrated
  2. washwashed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution and water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-26431e6a4a6c4a25a011ddb335f4ea16
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063234B2

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