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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 11613717, 화합물

HRID 1713999
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HRID 1713999 반응식
Cl.C(N=C=NCCCN(C)C)C.[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17]([NH2:20])(=[O:19])=[O:18].[CH:22]1([C:28]2[C:29]3[CH:30]=[CH:31][C:32]([C:50](O)=[O:51])=[CH:33][C:34]=3[N:35]3[CH2:42][CH2:41][N:40]([CH3:43])[CH2:39][C:38]4[CH:44]=[C:45]([O:48][CH3:49])[CH:46]=[CH:47][C:37]=4[C:36]=23)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17]([NH:20][C:50]([C:32]1[CH:31]=[CH:30][C:29]2[C:28]([CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[C:36]3[C:37]4[CH:47]=[CH:46][C:45]([O:48][CH3:49])=[CH:44][C:38]=4[CH2:39][N:40]([CH3:43])[CH2:41][CH2:42][N:35]3[C:34]=2[CH:33]=1)=[O:51])(=[O:19])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 21287077Methyl 2-sulfamoylacetateHCID 42640442HCID 42640442, 화합물

생성물 1

HCID 11613717HCID 11613717, 화합물수율 18%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6344
Dichloromethane
용매

실험 절차

1.6 eq of 1-ethyl-(3-dimethylaminopropyl)carbodiimide HCl salt was added to a mixture of 2.7 eq of DMAP, 1.6 eq of methyl(aminosulfonyl)acetate and the hydrochloride salt of 14-cyclohexyl-3-methoxy-6-methyl-5,6,7,8-tetrahydroindolo[2,1-a][2,5]-benzodiazocine-11-carboxylic acid (from Example 4) in DCM (0.02 M). The reaction was stirred at RT overnight before being partitioned between aqueous HCl (1 N) and EtOAc. The organics were washed with saturated aqueous NaHCO3, water and brine before being dried over Na2SO4, filtered and concentrated in vacuo. The crude was then purified by RP-HPLC (stationary phase: column Waters XTERRA prep. C18, 5 um, 30×50 mm. Mobile phase: MeCN/H2O buffered with 0.1% TFA). Fractions containing the pure compound were combined and freeze dried to afford the title compound as a white powder (18%).

후처리

  1. custombefore being partitioned between aqueous HCl (1 N) and EtOAc
  2. washThe organics were washed with saturated aqueous NaHCO3, water and brine
  3. dry with materialbefore being dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude was then purified by RP-HPLC (stationary phase: column Waters XTERRA prep. C18, 5 um, 30×50 mm. Mobile phase: MeCN/H2O buffered with 0.1% TFA)
  7. additionFractions containing the pure compound
  8. customfreeze dried

출처 및 근거

ORD 기록
ord-3ff17dbf438849369a2d81b324d52baa
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795247B2

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