Ethyl Acetate → HCID 67352373, 화합물

HRID 1672779노트

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HRID 1672779 반응식
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]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 67348151HCID 67348151, 화합물

생성물 1

HCID 67352373HCID 67352373, 화합물수율 33%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ff0c2666410a48d28841c1c5e41ec91f
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998954B2

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