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

HRID 636315

반응식

HRID 636315 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].[CH:41]1[C:54]2[C:53](=[O:55])[C:52]3[C:47](=[CH:48][CH:49]=[CH:50][CH:51]=3)[C:46](=[O:56])[C:45]=2[CH:44]=[CH:43][C:42]=1C(O)=O.C1CCC(N=C=NC2CCCCC2)CC1.C1C=CC2N(O)N=NC=2C=1.CN1CC[O:89][CH2:88]C1>C1COCC1.CN(C=O)C>[C:44]1([C:88]([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:89])[C:45]2[C:46](=[O:56])[C:47]3[C:52](=[CH:51][CH:50]=[CH:49][CH:48]=3)[C:53](=[O:55])[C:54]=2[CH:41]=[CH:42][CH:43]=1

참가 물질

8

반응물 5

HCID 79724-MethylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 670302-Anthraquinonecarboxylic acidHCID 757711-HydroxybenzotriazoleHCID 10555399HCID 10555399, 화합물

생성물 1

HCID 212573336-(1-Anthraquinonecarbonyl)-3,10-bis (2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicylo[10.3.1]hexadeca-1(16),12,14-triene수율 76%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

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 (1.0 g, 1.7 mmol), anthraquinone-2-carboxylic acid (0.43 g, 1.7 mmol), DCC (0.35 g, 1.7 mmol), HOBT (0.23 g, 1.7 mmol) and 4-methylmorpholine (0.25 g, 2.5 mmol) in 10 mL of anhydrous THF and 20 mL of anhydrous DMF in 56 h. The compound was purified by flash chromatography on a silica gel column using 200:1 CH2Cl2—MeOH as an eluent to give 1.06 g (76%) 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-45b22fedd8d549d0b0b74ce51cdd5c54
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191273B1

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