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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 46831860, 화합물

HRID 1518817
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HRID 1518817 반응식
[NH:1]1[C:9]2[C:4](=[C:5]([O:10][C:11]3[CH:19]=[C:18]([N:20]4[CH2:25][CH2:24][N:23]([CH:26]([C:28]5[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=5[C:34]5[CH:39]=[CH:38][C:37]([Cl:40])=[CH:36][CH:35]=5)[CH3:27])[CH2:22][CH2:21]4)[CH:17]=[CH:16][C:12]=3[C:13](O)=[O:14])[CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[N+:41]([C:44]1[CH:45]=[C:46]([S:58]([NH2:61])(=[O:60])=[O:59])[CH:47]=[CH:48][C:49]=1[NH:50][CH2:51][CH:52]1[CH2:57][CH2:56][O:55][CH2:54][CH2:53]1)([O-:43])=[O:42].Cl.C(N=C=NCCCN(C)C)C>CN(C)C1C=CN=CC=1.ClCCl>[Cl:40][C:37]1[CH:36]=[CH:35][C:34]([C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=2[CH:26]([N:23]2[CH2:22][CH2:21][N:20]([C:18]3[CH:17]=[CH:16][C:12]([C:13]([NH:61][S:58]([C:46]4[CH:47]=[CH:48][C:49]([NH:50][CH2:51][CH:52]5[CH2:53][CH2:54][O:55][CH2:56][CH2:57]5)=[C:44]([N+:41]([O-:43])=[O:42])[CH:45]=4)(=[O:59])=[O:60])=[O:14])=[C:11]([O:10][C:5]4[CH:6]=[CH:7][CH:8]=[C:9]5[C:4]=4[CH:3]=[CH:2][NH:1]5)[CH:19]=3)[CH2:25][CH2:24]2)[CH3:27])=[CH:39][CH:38]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 574749533-Nitro-4-(((tetrahydro-2H-pyran-4-yl) methyl)amino) benzene sulfonamideHCID 67227358HCID 67227358, 화합물

생성물 1

HCID 46831860HCID 46831860, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine
촉매
HCID 6344Dichloromethane용매

실험 절차

To a mixture of EXAMPLE 175E (66 mg), 3-nitro-4-((tetrahydro-2H-pyran-4-yl)methylamino)benzenesulfonamide (75 mg) and 4-dimethylaminopyridine (58.4 mg) in dichloromethane (5 mL) was added 1-ethyl-3-[3-(dimethylamino)propyl]-carbodiimide hydrochloride (45.8 mg). The mixture was stirred at ambient temperature overnight and concentrated. The concentrate was purified by RP HPLC (10-70% acetonitrile in 0.1% trifluoroacetic acid water/70 minutes). The desired fractions were concentrated to remove acetonitrile and the concentrate was diluted with dichloromethane and neutralized with aqueous NaHCO3. The dichloromethane layer was dried over Na2SO4 and concentrated to provide the title compound. 1H NMR (500 MHz, dimethysulfoxide-d6) δ ppm 11.31 (1H, s), 11.25 (1H, s), 8.62 (1H, t), 8.50 (1H, d), 7.68 (1H, dd), 7.53 (2H, d), 7.46 (2H, d), 7.37 (1H, t), 7.24-7.31 (4H, m), 7.17 (1H, d), 7.12 (1H, dd), 7.07 (1H, d), 6.96 (1H, t), 6.69 (1H, dd), 6.42 (1H, d), 6.26 (2H, s), 3.85 (2H, dd), 3.21-3.33 (5H, m), 3.01 (4H, s), 2.29-2.39 (2H, m), 2.15-2.22 (2H, m), 1.83-1.94 (1H, m), 1.57-1.68 (2H, m), 1.22-1.31 (2H, m), 1.17 (3H, d).

후처리

  1. concentrationconcentrated
  2. customThe concentrate was purified by RP HPLC (10-70% acetonitrile in 0.1% trifluoroacetic acid water/70 minutes)
  3. concentrationThe desired fractions were concentrated
  4. customto remove acetonitrile
  5. additionthe concentrate was diluted with dichloromethane and neutralized with aqueous NaHCO3
  6. dry with materialThe dichloromethane layer was dried over Na2SO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f9da81e789e042a0add9bed8e728bfc7
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09072748B2

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