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p-Toluenesulfonic acid monohydrate → HCID 56644098, 화합물

HRID 710226
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인쇄 미리보기

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HRID 710226 반응식
Cl.Cl[C:3]1[N:8]=[C:7]([NH:9][CH:10]2[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]2)[C:6]([F:20])=[CH:5][N:4]=1.[CH:21]([C:24]1[CH:29]=[CH:28][C:27]([NH2:30])=[CH:26][C:25]=1[N:31]1[CH:35]=[N:34][N:33]=[N:32]1)([CH3:23])[CH3:22].[OH2:36].C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(O)C>[NH3:4].[CH3:3][OH:36].[CH:21]([C:24]1[CH:29]=[CH:28][C:27]([NH:30][C:3]2[N:8]=[C:7]([NH:9][CH:10]3[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]3)[C:6]([F:20])=[CH:5][N:4]=2)=[CH:26][C:25]=1[N:31]1[CH:35]=[N:34][N:33]=[N:32]1)([CH3:23])[CH3:22]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 521998p-Toluenesulfonic acid monohydrateHCID 58065775HCID 58065775, 화합물HCID 86653878HCID 86653878, 화합물

생성물 2

HCID 21705897Ammonia methanolHCID 56644098HCID 56644098, 화합물수율 106.9%

시약·촉매·용매 1

HCID 3776Isopropanol
용매

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온도
100 °C

실험 절차

A mixture of 2-chloro-5-fluoro-N-(2,2,6,6-tetramethylpiperidin-4-yl)pyrimidin-4-amine hydrochloride (160 mg, 0.495 mmol, 1 equiv), 4-isopropyl-3-(1H-tetrazol-1-yl)benzenamine (121 mg, 0.594 mmol, 1.2 equiv), and para-toluenesulfonic acid monohydrate (75 mg, 0.396 mmol, 0.8 equiv) in IPA (3 mL) were heated to 100° C. for 3 hours. After cooling to ambient temperature, the crude mixture was quenched with 2M NH3/MeOH followed by concentrating to dryness. The crude product was purified by flash chromatography and eluted with DCM:2M NH3/MeOH (95:5) to provide the desired product (120 mg, 54%) as a white solid.

후처리

  1. temperatureAfter cooling to ambient temperature
  2. customthe crude mixture was quenched with 2M NH3/MeOH
  3. concentrationby concentrating to dryness
  4. customThe crude product was purified by flash chromatography
  5. washeluted with DCM

출처 및 근거

ORD 기록
ord-ae8afdd4c2f24a069e082031ba915ea4
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181222B2

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