2,2-Dimethyl-1,3-dioxane-4,6-dione → HCID 58392263、化合物

HRID 561380

反応式

HRID 561380 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 58392263HCID 58392263、化合物収率 103.9%

試薬・触媒・溶媒 2

HCID 614proline dl-form触媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-26431e6a4a6c4a25a011ddb335f4ea16
出典データセット
uspto-grants-2011_11
特許番号
US08063234B2

関連ノート

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