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1-Hydroxybenzotriazole → [3-(2-Amino-4,5-dimethoxy-phenylcarbamoyl)-propyl]-methyl-carbamic acid benzyl ester

HRID 220239
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HRID 220239 반응식
[CH2:1]([O:8][C:9]([N:11]([CH3:18])[CH2:12][CH2:13][CH2:14][C:15]([OH:17])=O)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.C1C=CC2N(O)N=NC=2C=1.Cl.Cl.[CH3:40][O:41][C:42]1[CH:43]=[C:44]([NH2:51])[C:45]([NH2:50])=[CH:46][C:47]=1[O:48][CH3:49].C([O-])(O)=O.[Na+]>C1COCC1.C(Cl)CCl>[CH2:1]([O:8][C:9](=[O:10])[N:11]([CH2:12][CH2:13][CH2:14][C:15](=[O:17])[NH:50][C:45]1[CH:46]=[C:47]([O:48][CH3:49])[C:42]([O:41][CH3:40])=[CH:43][C:44]=1[NH2:51])[CH3:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

8

반응물 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 130002194,5-Dimethoxybenzene-1,2-diamine--hydrogen chloride (1/2)HCID 190283044-(((Benzyloxy)carbonyl)(methyl)amino)butanoic acid

생성물 1

HCID 68414218
[3-(2-Amino-4,5-dimethoxy-phenylcarbamoyl)-propyl]-methyl-carbamic acid benzyl ester

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 0.95 g 4-(benzyloxycarbonyl-methyl-amino)-butyric acid in 20 mL THF were added 3.3 mL of DIPEA, 0.61 g of HOBt and 0.86 g EDC. After stirring for 5 min 1.0 g of 4,5-dimethoxy-benzene-1,2-diamine dihydrochloride was added and the mixture was stirred at rt overnight. Saturated aq. NaHCO3 solution was added, the phases were separated and the organic phase was washed with brine. The combined organic phases were dried over MgSO4, and concentrated in vacuo.

후처리

  1. additionwas added
  2. customthe phases were separated
  3. washthe organic phase was washed with brine
  4. dry with materialThe combined organic phases were dried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22ca4ff8a7674726a83415621108f133
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202885B2

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