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Hydrochloride methanol → HCID 67959638, 화합물

HRID 1529359
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HRID 1529359 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[N:20]=[C:19]([C:21]3[C:29]4[C:24](=[CH:25][CH:26]=[C:27]([NH:30]C(=O)CC)[CH:28]=4)[N:23](C(OC(C)(C)C)=O)[CH:22]=3)[CH:18]=[N:17][CH:16]=2)[CH2:11][CH2:10]1)=O)(C)(C)C.CO.Cl>>[NH2:8][CH:9]1[CH2:10][CH2:11][N:12]([C:15]2[N:20]=[C:19]([C:21]3[C:29]4[C:24](=[CH:25][CH:26]=[C:27]([NH2:30])[CH:28]=4)[NH:23][CH:22]=3)[CH:18]=[N:17][CH:16]=2)[CH2:13][CH2:14]1
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참가 물질

3

반응물 2

HCID 21893726Hydrochloride methanolHCID 67958305HCID 67958305, 화합물

생성물 1

HCID 67959638HCID 67959638, 화합물수율 31.2%

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온도
60 °C

실험 절차

A mixture of tert-butyl 3-(6-(4-(tert-butoxycarbonylamino)piperidin-1-yl)pyrazin-2-yl)-5-propionamido-1H-indole-1-carboxylate (150 mg, 0.26 mmol) and 3 N MeOH—HCl (3 mL) was stirred at 60° C. overnight. The reaction mixture was quenched with water and neutralized with K2CO3. The resulting precipitate was filtered, washed with water and dried to obtain the crude product. The crude product was purified by prep HPLC (column: Zorbax Eclipse XDBC Prep C18 5 μm 21.2*150 mm; flow rate: 15.0 mL/min; mobile phase: A: 0.1% TFA in water. B: ACN+MeOH (1:1); gradient: % B, 10% to 50%) to obtain the title compound (25 mg, 28%). MS (ESI, pos. ion) m/z: 309.1 (M+1).

후처리

  1. customThe reaction mixture was quenched with water and neutralized with K2CO3
  2. filtrationThe resulting precipitate was filtered
  3. washwashed with water
  4. customdried
  5. customto obtain the crude product
  6. customThe crude product was purified by prep HPLC (column

출처 및 근거

ORD 기록
ord-6c1040dfce504b7594dae039b4223b5e
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09090593B2

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