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

Hydrazine → HCID 178434214, 화합물

HRID 2367480
노트
인쇄 미리보기

반응식

HRID 2367480 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:15]=[C:14]([NH2:16])[N:13]=[C:12]([N:17]3[C@H:22]([CH3:23])[CH2:21][CH2:20][C@H:19]([C:24]([NH:26][CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[O:25])[CH2:18]3)[CH:11]=2)=[CH:6][C:5]=1F)(=O)[CH3:2].Cl.CON.C([O-])([O-])=O.[K+].[K+].CCN(C(C)C)C(C)C.[NH2:54][NH2:55]>COCCOC.CCO>[NH2:16][C:14]1[N:13]=[C:12]([N:17]2[C@H:22]([CH3:23])[CH2:21][CH2:20][C@H:19]([C:24]([NH:26][CH2:27][C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)=[O:25])[CH2:18]2)[CH:11]=[C:10]([C:7]2[CH:6]=[C:5]3[C:4]([C:1]([CH3:2])=[N:54][NH:55]3)=[CH:9][CH:8]=2)[N:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 9321HydrazineHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 58504436(3S,6R)-1-[6-(4-Acetyl-3-fluorophenyl)-2-amino-4-pyrimidinyl]-6-methyl-N-(phenylmethyl)-3-piperidinecarboxamide

생성물 1

HCID 178434214HCID 178434214, 화합물
수율 10.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
120 °C

실험 절차

Into a sealed tube, (3S,6R)-1-[6-(4-acetyl-3-fluorophenyl)-2-amino-4-pyrimidinyl]-6-methyl-N-(phenylmethyl)-3-piperidinecarboxamide (90 mg, 0.195 mmol), O-methylhydroxylamine hydrochloride (16.3 mg, 0.20 mmol), and K2CO3 (32.3 mg, 0.234 mmol) were stirred together in DME (3 mL) for 4 hours at 57° C. The reaction mixture was filtered, and the filtrate containing the oxime intermediate was concentrated in vacuo to 2 mL. Then EtOH (3 mL), Hunig's base (0.05 mL, 0.27 mmol), and hydrazine anhydrous (0.013 mL, 0.410 mmol) were added, and the resulting yellow mixture was heated overnight at 120° C. in an oil bath. The solution turned black. LCMS showed mainly product. The black solid was filtered and the yellow filtrate was evaporated. The resulting yellow residue was dissolved in CH3OH, and purified by HPLC (CH3CN/H2O w/0.1% HCO2H) to afford a formic acid salt of the title compound (9 mg) as a light yellow solid. LC-MS (ES) m/z=456 [M+H]+. 1H NMR (400 MHz, CD3OD): δ 1.32 (m, 4H), 1.75-1.91 (m, 3H), 1.97-2.12 (m, 1H), 2.41-2.53 (m, 1H), 2.60 (s, 3H), 3.11-3.27 (m, 1H), 4.33-4.50 (m, 2H), 4.56-4.74 (m, 1H), 6.59 (s, 1H), 7.23-7.41 (m, 5H), 7.54-7.63 (m, 1H), 7.96 (m, 1H), 7.94 (s, 1H).

후처리

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate containing the oxime intermediate
  3. concentrationwas concentrated in vacuo to 2 mL
  4. filtrationThe black solid was filtered
  5. customthe yellow filtrate was evaporated
  6. dissolutionThe resulting yellow residue was dissolved in CH3OH
  7. custompurified by HPLC (CH3CN/H2O w/0.1% HCO2H)

출처 및 근거

ORD 기록
ord-62ac067d1f7748aa89b22baa3f87345f
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