4-Methylmorpholine → 6-(1-Pyrenecarbonyl)-3,10-bis(2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicyclo[10.3.1]hexadeca-1(16),12,14-triene

HRID 636316

반응식

HRID 636316 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([N:13]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23][CH2:22][N:21]([S:28]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=2[N+:37]([O-:39])=[O:38])(=[O:30])=[O:29])[CH2:20][C:19]2[N:40]=[C:15]([CH:16]=[CH:17][CH:18]=2)[CH2:14]1)(=[O:12])=[O:11])([O-:3])=[O:2].[C:41]1([C:57](O)=[O:58])[C:54]2[C:55]3=[C:56]4[C:51](=[CH:52][CH:53]=2)[CH:50]=[CH:49][CH:48]=[C:47]4[CH:46]=[CH:45][C:44]3=[CH:43][CH:42]=1.C1CCC(N=C=NC2CCCCC2)CC1.C1C=CC2N(O)N=NC=2C=1.CN1CCOCC1>C(Cl)Cl.CN(C=O)C>[C:41]1([C:57]([N:25]2[CH2:24][CH2:23][CH2:22][N:21]([S:28]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=3[N+:37]([O-:39])=[O:38])(=[O:30])=[O:29])[CH2:20][C:19]3[N:40]=[C:15]([CH:16]=[CH:17][CH:18]=3)[CH2:14][N:13]([S:10]([C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=3[N+:1]([O-:3])=[O:2])(=[O:12])=[O:11])[CH2:27][CH2:26]2)=[O:58])[C:54]2[C:55]3=[C:56]4[C:51](=[CH:52][CH:53]=2)[CH:50]=[CH:49][CH:48]=[C:47]4[CH:46]=[CH:45][C:44]3=[CH:43][CH:42]=1

참가 물질

8

반응물 5

HCID 79724-MethylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 1253951-Pyrenecarboxylic acidHCID 10555399HCID 10555399, 화합물

생성물 1

HCID 108192156-(1-Pyrenecarbonyl)-3,10-bis(2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicyclo[10.3.1]hexadeca-1(16),12,14-triene수율 86%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

The title compound was prepared following the procedures illustrated above in Example 75 using 3,10-bis(2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicyclo-[10.3.1]hexadeca-1(16),12,14-triene (0.59 g, 1.0 mmol), 1-pyrenecarboxylic acid (0.25 g, 1.0 mmol), DCC (0.21 g, 1.0 mmol), HOBT (0.14 g, 1.0 mmol) and 4-methylmorpholine (0.15 g, 1.5 mmol) in 20 mL of CH2Cl2 and 10 mL of DMF. The compound was purified by flash chromatography on a silica gel column using 200:1 CH2Cl2—MeOH as an eluent to give 0.7 g (86%) of the title compound as a pale yellow foam.

후처리

  1. customThe title compound was prepared
  2. customThe compound was purified by flash chromatography on a silica gel column

출처 및 근거

ORD 기록
ord-b15a08b888f7409ab327a94b1cea0a45
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191273B1

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