1,2-Dichloroethane → HCID 70234737, 화합물

HRID 2098459노트

반응식

HRID 2098459 반응식
[CH3:1][C:2]([O:5][C:6]([NH:8][C@H:9]([C:14]([OH:16])=O)[C:10]([CH3:13])([CH3:12])[CH3:11])=[O:7])([CH3:4])[CH3:3].[C@H:17]12[CH2:23][C@H:20]([NH:21][CH2:22]1)[CH2:19][N:18]2[C:24]([C:26]1[NH:30][C:29]2[CH:31]=[CH:32][CH:33]=[CH:34][C:28]=2[N:27]=1)=[O:25].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CN1CCOCC1>C(Cl)Cl.O>[NH:27]1[C:28]2[CH:34]=[CH:33][CH:32]=[CH:31][C:29]=2[N:30]=[C:26]1[C:24]([N:18]1[CH2:19][C@@H:20]2[CH2:23][C@H:17]1[CH2:22][N:21]2[C:14]([C@@H:9]([NH:8][C:6](=[O:7])[O:5][C:2]([CH3:1])([CH3:3])[CH3:4])[C:10]([CH3:11])([CH3:12])[CH3:13])=[O:16])=[O:25]

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 2734668(S)-2-((tert-Butoxycarbonyl)amino)-3,3-dimethylbutanoic acidHCID 58286559HCID 58286559, 화합물

생성물 1

HCID 70234737HCID 70234737, 화합물수율 99.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

A solution of N-{[(1,1-dimethylethyl)oxy]carbonyl}-3-methyl-L-valine (3 g, 13 mmol) (2-[(1S,4S)-2,5-diazabicyclo[2.2.1]hept-2-ylcarbonyl]-1H-benzimidazole (3 g, 12.4 mmol), EDC (2.8 g, 14.8 mmol), HOBt (334 mg, 2.5 mmol), NMM (3.7 g, 37.1 mmol) in CH2Cl2 (50 mL) was stirred at room temperature for 18 h. The reaction was diluted with water and CH2Cl2 then washed with sat. NaHCO3 (50 mL) and brine (50 mL). The solution was dried over anhydrous Na2SO4 and concentrated to give the title compound (5.6 g) as a pale yellow solid. LCMS (m/z): 456.3 (M+H).

후처리

  1. washthen washed with sat. NaHCO3 (50 mL) and brine (50 mL)
  2. dry with materialThe solution was dried over anhydrous Na2SO4
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-761bb1373f174e769e46c18e9216385a
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450484B2

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