Ethyl Acetate → HCID 67352373、化合物

HRID 1672779ノート

反応式

HRID 1672779 の反応式
C([O:4][CH2:5][C:6]1[O:10][C:9]([C:11]2[CH:12]=[C:13]([N:17]3[CH2:26][C@H:25]4[N:21]([CH2:22][CH2:23][CH2:24]4)[C:20]4[N:27]=[C:28]([NH:31][CH2:32][CH3:33])[N:29]=[CH:30][C:19]=4[C:18]3=[O:34])[CH:14]=[CH:15][CH:16]=2)=[N:8][N:7]=1)(=O)C.[OH-].[Na+].C(OCC)(=O)C>CO>[CH2:32]([NH:31][C:28]1[N:29]=[CH:30][C:19]2[C:18](=[O:34])[N:17]([C:13]3[CH:14]=[CH:15][CH:16]=[C:11]([C:9]4[O:10][C:6]([CH2:5][OH:4])=[N:7][N:8]=4)[CH:12]=3)[CH2:26][C@H:25]3[N:21]([CH2:22][CH2:23][CH2:24]3)[C:20]=2[N:27]=1)[CH3:33]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 67348151HCID 67348151、化合物

生成物 1

HCID 67352373HCID 67352373、化合物収率 33%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(S)-5-[3-(5-Acetoxymethyl-1,3,4-oxadiazol-2-yl)phenyl]-9-ethylamino-1,2,3,3a,4,5-hexahydro-5,8,10,10b-tetraazabenzo[e]azulen-6-one (20.0 mg, 0.0432 mmol) obtained in Step 1 was dissolved in methanol (2 mL), and the mixture was stirred at room temperature for 30 minutes after adding a 1 mol/L aqueous sodium hydroxide solution (2 mL). The mixture was diluted by addition of ethyl acetate, and washed with water. The organic layer was dried over anhydrous magnesium sulfate, concentrated under reduced pressure, and crystallized from diisopropylether to give the title compound (Compound 48) (6.0 mg, 33%).

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customcrystallized from diisopropylether

出典と根拠

ORDレコード
ord-ff0c2666410a48d28841c1c5e41ec91f
出典データセット
uspto-grants-2011_08
特許番号
US07998954B2

反応ノート

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