홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethanol → (3S,6R)-1-[2-Amino-6-(3-amino-1H-indazol-6-yl)-4-pyrimidinyl]-6-methyl-N-{[3-(methyloxy)phenyl]methyl}-3-piperidinecarboxamide

HRID 2367584
노트
인쇄 미리보기

반응식

HRID 2367584 반응식
[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[C@H:13]([CH3:14])[CH2:12][CH2:11][C@H:10]([C:15]([NH:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH3:26])[CH:20]=3)=[O:16])[CH2:9]2)[CH:5]=[C:4]([C:27]2[CH:32]=[CH:31][C:30]([C:33]#[N:34])=[C:29](F)[CH:28]=2)[N:3]=1.CCO.CCN(C(C)C)C(C)C.[NH2:48][NH2:49]>CO>[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[C@H:13]([CH3:14])[CH2:12][CH2:11][C@H:10]([C:15]([NH:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH3:26])[CH:20]=3)=[O:16])[CH2:9]2)[CH:5]=[C:4]([C:27]2[CH:28]=[C:29]3[C:30]([C:33]([NH2:34])=[N:48][NH:49]3)=[CH:31][CH:32]=2)[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 9321HydrazineHCID 81531DiisopropylethylamineHCID 58504830HCID 58504830, 화합물

생성물 1

HCID 46214815(3S,6R)-1-[2-Amino-6-(3-amino-1H-indazol-6-yl)-4-pyrimidinyl]-6-methyl-N-{[3-(methyloxy)phenyl]methyl}-3-piperidinecarboxamide수율 16.3%

시약·촉매·용매 1

HCID 887
Methanol
용매

반응 조건

온도
110 °C

실험 절차

Into a sealable tube, (3S,6R)-1-[2-amino-6-(4-cyano-3-fluorophenyl)-4-pyrimidinyl]-6-methyl-N-{[3-(methyloxy)phenyl]methyl}-3-piperidinecarboxamide (186 mg, 0.392 mmol), EtOH (5 mL), Hunig's base (0.068 ml, 0.392 mmol), and hydrazine anhydrous (0.074 mL, 2.35 mmol) were added, and the yellow suspension mixture was heated overnight at 110° C. in an oil bath. When the temperature of the reaction reached to 100° C., the solid in the mixture was all dissolved. After overnight, there was a yellow solution as well as a little amount of black colored solid formed. LCMS showed mainly product. CH3OH (5 mL) was added to the solution. The black solid was filtered from the yellow solution. Water (20 mL) was added to the yellow solution, and a solid was formed. The solid was filtered, washed by water, and dried in vacuum. The solid was recrystallized from CH3CN, and the solid was filtered, washed by CH3CN, and dried in vacuum to afford the title compound (31 mg) as a light yellow solid. LC-MS (ES) m/z=487 [M+H]+. 1H NMR (400 MHz, DMSO-d6): δ 1.16 (d, J=6.8 Hz, 3H), 1.58-1.71 (m, 2H), 1.76 (m, 1H), 1.86 (m, 1H), 2.36 (m, 1H), 3.75 (s, 3H), 4.19 (m, 1H), 4.23 (m, 1H), 4.33 (m, 1H), 4.37 (m, 1H), 5.38 (s, 2H), 6.08 (s, 2H), 6.59 (s, 1H), 6.81-6.91 (m, 3H), 7.26 (m, 1H), 7.52-7.63 (m, 1H), 7.70 (d, J=8.6 Hz, 1H), 7.94 (s, 1H), 8.48 (m, 1H), 11.50 (s, 1H).

후처리

  1. customreached to 100° C.
  2. customformed
  3. filtrationThe black solid was filtered from the yellow solution
  4. additionWater (20 mL) was added to the yellow solution
  5. customa solid was formed
  6. filtrationThe solid was filtered
  7. washwashed by water
  8. customdried in vacuum
  9. customThe solid was recrystallized from CH3CN
  10. filtrationthe solid was filtered
  11. washwashed by CH3CN
  12. customdried in vacuum

출처 및 근거

ORD 기록
ord-290079de84b24b93862ba316a5384dcf
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697685B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트