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HCID 59713612, 화합물 → HCID 10312102, 화합물

HRID 2223080
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HRID 2223080 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[CH:9]([N:14]=[C:15]=[S:16])[N:8]=[C:7]([C:17]3[CH:21]=[CH:20][S:19][CH:18]=3)[C:6]=2[CH:22]=1.[N:23]1([C:29]2[C:38]3[C:33](=[CH:34][CH:35]=[CH:36][CH:37]=3)[C:32]([NH2:39])=[CH:31][CH:30]=2)[CH2:28][CH2:27][O:26][CH2:25][CH2:24]1>CC(N(C)C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[CH:9]([NH:14][C:15]([NH:39][C:32]3[C:33]4[C:38](=[CH:37][CH:36]=[CH:35][CH:34]=4)[C:29]([N:23]4[CH2:28][CH2:27][O:26][CH2:25][CH2:24]4)=[CH:30][CH:31]=3)=[S:16])[N:8]=[C:7]([C:17]3[CH:21]=[CH:20][S:19][CH:18]=3)[C:6]=2[CH:22]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 59713612HCID 59713612, 화합물HCID 59713770HCID 59713770, 화합물

생성물 1

HCID 10312102HCID 10312102, 화합물

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
70 °C

실험 절차

This reaction was carried out in a multiwell plate. As illustrated in the scheme above, aA mixture of 7-chloro-1,3-dihydro-3-isothiocyanato-1-methyl-5-(3-thienyl)-2H-1,4-benzodiazepin-2-one (156 μL of a 0.128 M solution in (CH2Cl)2, 0.020 mmol), 4-(4-morpholinyl)-1-naphthalenamine (44 μL of a 0.5 M solution in DMA, 0.022 mmol), and (CH2Cl)2 (300 μL) was agitated and heated at 70° C. for 22 h. The reaction was cooled and concentrated in vacuo, and the residue was redissolved in DMA (25 μL) and (CH2Cl)2 (275 μL). Polyamine resin HL (NovaBiochem) was added (20 mg of 4.53 mmol/g, 0.091 mmol), and the mixture was agitated at room temperature overnight. The resin was removed by filtration and washed with additional (CH2Cl)2 and MeOH. The filtrate was concentrated in vacuo to provide the title compound. MS (ESI) (M+H)+=576.

후처리

  1. temperatureThe reaction was cooled
  2. concentrationconcentrated in vacuo
  3. dissolutionthe residue was redissolved in DMA (25 μL)
  4. additionPolyamine resin HL (NovaBiochem) was added (20 mg of 4.53 mmol/g, 0.091 mmol)
  5. stirringthe mixture was agitated at room temperature overnight
  6. customThe resin was removed by filtration
  7. washwashed with additional (CH2Cl)2 and MeOH
  8. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-66c615f5ea2648a8b725a41470633117
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07375101B2

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