Ethyl Acetate → HCID 9947145、化合物

HRID 382466ノート

反応式

HRID 382466 の反応式
C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C.C([C@@H]([C@H](C(O)=O)O)O)(O)=O.[C:23]([O:31][CH2:32][CH2:33][CH2:34][N:35]1[C:43]2[C:38](=[CH:39][C:40]([CH2:46][C@H:47]([NH2:49])[CH3:48])=[CH:41][C:42]=2[C:44]#[N:45])[CH2:37][CH2:36]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>O>[C:23]([O:31][CH2:32][CH2:33][CH2:34][N:35]1[C:43]2[C:38](=[CH:39][C:40]([CH2:46][C@H:47]([NH2:49])[CH3:48])=[CH:41][C:42]=2[C:44]#[N:45])[CH2:37][CH2:36]1)(=[O:30])[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 45108224(2R,3R)-2,3-Dihydroxybutanedioic acid--3-{5-[(2R)-2-aminopropyl]-7-cyano-2,3-dihydro-1H-indol-1-yl}propyl benzoate (1/1)

生成物 1

HCID 9947145HCID 9947145、化合物収率 105.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of potassium carbonate (32.3 g) in distilled water(120 ml) was added ethyl acetate (120 ml), and (R)-3-[5-(2-aminopropyl)-7-cyano-2,3-dihydro-1H-indol-1-yl]propyl benzoate L-tartrate (12.0 g) was added portionwise to the mixture with stirring. After reaction for 1 hour, the reaction mixture was extracted with ethyl acetate, and the ethyl acetate layer was washed with 10% aqueous potassium carbonate solution and brine subsequently, and dried over anhydrous sodium sulfate. The solvent was removed in vacuo to give (R)-3-[5-(2-aminopropyl)-7-cyano-2,3-dihydro-1H-indol-1-yl]propyl benzoate (8.98 g) as a brown oil.

後処理

  1. additionwas added portionwise to the mixture
  2. customAfter reaction for 1 hour
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washthe ethyl acetate layer was washed with 10% aqueous potassium carbonate solution and brine subsequently
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-88d2bfca419a4061a60d592948c85c44
出典データセット
uspto-grants-2001_10
特許番号
US06310086B1

反応ノート

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