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Hydrochloric Acid → HCID 86699013, 화합물

HRID 1520075
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HRID 1520075 반응식
[ClH:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[N:12]=[N:13][N:14]([C:16]3[CH:21]=[CH:20][C:19]([C:22]4[CH2:23][CH2:24][N:25]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:26][CH:27]=4)=[CH:18][CH:17]=3)[CH:15]=2)=[N:3]1>O1CCOCC1>[ClH:1].[NH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]2[N:12]=[N:13][N:14]([C:16]3[CH:17]=[CH:18][C:19]([C:22]4[CH2:23][CH2:24][N:25]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:26][CH:27]=4)=[CH:20][CH:21]=3)[CH:15]=2)=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 67981119HCID 67981119, 화합물

생성물 1

HCID 86699013HCID 86699013, 화합물수율 87.7%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

Hydrogen chloride (6.0 mL of a 4N solution in dioxane) was added to a suspension of tert-butyl 4-{4-[4-(1H-indazol-3-yl)-1H-1,2,3-triazol-1-yl]phenyl}-3,6-dihydropyridine-1(2H)-carboxylate (505 mg; 1.14 mmol; 1.0 eq.) in Dioxane (6.0 mL). The resulting light brown suspension was stirred at 350 for 3 h. It was then concentrated to dryness and the resulting beige solid was suspended in dioxane, filtered, rinsed several times with Et2O and dried under vacuum at 400 to give the title compound as a beige solid (379 mg; 87.7%). 1H NMR (300 MHz, DMSO-d6) δ 13.43 (brs, 1H), 9.52-9.14 (m, 3H), 8.36 (d, J=8.1, 1H), 8.10 (d, J=8.0, 2H), 7.75 (d, J=8.1, 2H), 7.62 (d, J=8.5, 1H), 7.44 (t, J=7.6, 1H), 7.26 (t, J=7.2, 1H), 6.37 (s, 1H), 3.96-3.67 (m, 2H), 3.45-3.18 (m, 2H), 2.93-2.57 (m, 2H).

후처리

  1. concentrationIt was then concentrated to dryness
  2. filtrationfiltered
  3. washrinsed several times with Et2O
  4. customdried under vacuum at 400

출처 및 근거

ORD 기록
ord-68f9885a042944d68fb8bb3ac9711e8a
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073892B2

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