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Morpholine → HCID 44540962, 화합물

HRID 1616021
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HRID 1616021 반응식
[Cl:1][C:2]1[C:3]([C:9]([NH:11][C:12]2[CH:20]=[C:19]([C:21]3[CH:29]=[CH:28][CH:27]=[C:26]4[C:22]=3[CH:23]=[CH:24][NH:25]4)[CH:18]=[C:17]3[C:13]=2[CH:14]=[N:15][NH:16]3)=[O:10])=[N:4][C:5](Cl)=[CH:6][CH:7]=1.[NH:30]1[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1.CCN(C(C)C)C(C)C>CS(C)=O.CS(C)=O.CO>[Cl:1][C:2]1[C:3]([C:9]([NH:11][C:12]2[CH:20]=[C:19]([C:21]3[CH:29]=[CH:28][CH:27]=[C:26]4[C:22]=3[CH:23]=[CH:24][NH:25]4)[CH:18]=[C:17]3[C:13]=2[CH:14]=[N:15][NH:16]3)=[O:10])=[N:4][C:5]([N:30]2[CH2:35][CH2:34][O:33][CH2:32][CH2:31]2)=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 44540871HCID 44540871, 화합물

생성물 1

HCID 44540962HCID 44540962, 화합물수율 16.1%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 22036561Dimethyl sulfoxide methanol
용매

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온도
160 °C

실험 절차

To a microwave vial was added 2 ml of a solution of 3,6-dichloro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-2-pyridinecarboxamide (306 mg, 0.71 mmol) in DMSO (6 ml). Morpholine (0.022 ml, 0.25 mmol) and DIPEA (0.129 ml) were added and the mixture was heated at 160° C. for 3 h under microwave irradiation. The crude reaction mixture was dissolved in DMSO/MeOH (1:1) and purified by Mass Directed Automated Preparative HPLC (Method E). The sample was further purified by Mass Directed Automated Preparative HPLC (Method E) and product-containing fractions were dried under a stream of nitrogen to afford the title compound (19 mg).

후처리

  1. customThe crude reaction mixture
  2. custompurified by Mass Directed Automated Preparative HPLC (Method E)
  3. customThe sample was further purified by Mass Directed Automated Preparative HPLC (Method E)
  4. additionproduct-containing fractions
  5. customwere dried under a stream of nitrogen

출처 및 근거

ORD 기록
ord-67c66db6fde742eb86f6dffa2ab92abf
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765743B2

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