Hydrochloric Acid → HCID 178462798, 화합물

HRID 1401231노트

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HRID 1401231 반응식
[CH2:1]([N:3]1[C:12]2[C:7](=[N:8][CH:9]=[C:10]([C:13]3[CH:18]=[CH:17][C:16]([C:19]4[N:23](C5CCCCO5)[CH:22]=[N:21][N:20]=4)=[CH:15][CH:14]=3)[N:11]=2)[NH:6][C:5](=[O:30])[CH2:4]1)[CH3:2].[ClH:31]>C(O)C.O1CCOCC1>[ClH:31].[N:21]1[N:20]=[C:19]([C:16]2[CH:17]=[CH:18][C:13]([C:10]3[N:11]=[C:12]4[N:3]([CH2:1][CH3:2])[CH2:4][C:5](=[O:30])[NH:6][C:7]4=[N:8][CH:9]=3)=[CH:14][CH:15]=2)[NH:23][CH:22]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 666071504-Ethyl-6-(4-(4-(tetrahydro-2H-pyran-2-yl)-4H-1,2,4-triazol-3-yl)phenyl)-3,4-dihydro-pyrazino[2,3-b]pyrazin-2(1H)-one

생성물 1

HCID 178462798HCID 178462798, 화합물수율 82%

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 312751,4-Dioxane용매

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온도
75 °C

실험 절차

4-Ethyl-6-(4-(4-(tetrahydro-2H-pyran-2-yl)-4H-1,2,4-triazol-3-yl)phenyl)-3,4-dihydropyrazino[2,3-b]pyrazin-2(1H)-one in ethanol was treated with 2 N hydrogen chloride in dioxane. The solution was stirred at 75° C. for 1 h. The solution was condensed partially and cooled. Cold ethanol was added to the slurry and the resulting precipitate filtered and washed with additional cold ethanol followed by hexanes to afford the title compound as the hydrochloride salt in 82% yield. 1H NMR (400 MHz, METHANOL-d4) δ (ppm) 9.18 (s, 1H), 8.22 (d, J=8.59 Hz, 2H), 8.04-8.09 (m, 3H), 7.66-7.74 (m, 1H), 7.58-7.64 (m, 1H), 4.24 (s, 2H), 3.74 (q, J=7.03 Hz, 2H), 1.29 (t, J=7.03 Hz, 4H), 0.79-0.98 (m, 4H); MS (ESI) m/z 322.2 [M+1]+.

후처리

  1. customcondensed partially
  2. temperaturecooled
  3. filtrationthe resulting precipitate filtered
  4. washwashed with additional cold ethanol

출처 및 근거

ORD 기록
ord-4f9cde4a3be043479d3b1e29c07b94af
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907087B2

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