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Ammonia methanol → HCID 89484446, 화합물

HRID 2283665
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HRID 2283665 반응식
[NH3:1].CO.[S:4]1[CH:8]=[CH:7][C:6]2[C:9]([NH:13][C:14]3[N:15]=[C:16]([NH:25][C@@H:26]4[CH2:31][CH2:30][CH2:29][CH2:28][C@@H:27]4[NH:32]C(OC(C)(C)C)=O)[N:17]=[N:18][C:19]=3[C:20](OCC)=[O:21])=[CH:10][CH:11]=[CH:12][C:5]1=2>>[NH2:32][C@H:27]1[CH2:28][CH2:29][CH2:30][CH2:31][C@H:26]1[NH:25][C:16]1[N:17]=[N:18][C:19]([C:20]([NH2:1])=[O:21])=[C:14]([NH:13][C:9]2[C:6]3[CH:7]=[CH:8][S:4][C:5]=3[CH:12]=[CH:11][CH:10]=2)[N:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 21705897Ammonia methanolHCID 90308809HCID 90308809, 화합물

생성물 1

HCID 89484446HCID 89484446, 화합물

실험 절차

A 7 M ammonia-methanol solution (2 ml) was added to ethyl 5-(benzo[b]thiophen-4-ylamino)-3-((1R,2S)-2-(tert-butoxycarbonylamino)cyclohexylamino)-1,2,4-triazine-6-carboxylate obtained in the above-described Step 2 (71.8 mg), and then the reaction solution was allowed to react in a microwave reactor at 130° C. for 1 hour. The solvent was evaporated under vacuum, then trifluoroacetic acid (0.5 ml) was added to the resultant residue, and the reaction solution was stirred at room temperature for 5 minutes. The solvent was evaporated under vacuum, and then the resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate) to obtain the titled compound as a white solid.

후처리

  1. customobtained in the above-described Step 2 (71.8 mg)
  2. customto react in a microwave reactor at 130° C. for 1 hour
  • customThe solvent was evaporated under vacuum
  • additiontrifluoroacetic acid (0.5 ml) was added to the resultant residue
  • customThe solvent was evaporated under vacuum
  • customthe resultant residue was purified by column chromatography on basic silica gel (developing solvent:hexane/ethyl acetate)
  • 출처 및 근거

    ORD 기록
    ord-8b8c850fcb9a4a0fb05cc896e19e518b
    출처 데이터셋
    uspto-grants-2015_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US09145414B2

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