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

Hydrochloric Acid → 4-(1-Ethyl-3,5-dimethyl-1H-pyrazol-4-ylmethyl)-3'-(4-fluoro-phenyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl hydrochloride

HRID 220524
노트
인쇄 미리보기

반응식

HRID 220524 반응식
[ClH:1].Cl.[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[C:11]([N:16]3[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]3)=[N:12][CH:13]=[CH:14][N:15]=2)=[CH:6][CH:5]=1.[CH2:22]([N:24]1[C:28]([CH3:29])=[C:27]([CH:30]=O)[C:26]([CH3:32])=[N:25]1)[CH3:23].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+].Cl>O1CCCC1.C(#N)C.C(Cl)Cl>[ClH:1].[CH2:22]([N:24]1[C:28]([CH3:29])=[C:27]([CH2:30][N:19]2[CH2:18][CH2:17][N:16]([C:11]3[C:10]([C:7]4[CH:8]=[CH:9][C:4]([F:3])=[CH:5][CH:6]=4)=[N:15][CH:14]=[CH:13][N:12]=3)[CH2:21][CH2:20]2)[C:26]([CH3:32])=[N:25]1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 31574611-Ethyl-3,5-dimethyl-1H-pyrazole-4-carbaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 673669583'-(4-fluoro-phenyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl dihydrochloride

생성물 1

HCID 68596950
4-(1-Ethyl-3,5-dimethyl-1H-pyrazol-4-ylmethyl)-3'-(4-fluoro-phenyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl hydrochloride
수율 15%

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred suspension of 3′-(4-fluoro-phenyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl dihydrochloride (0.3 g, 0.906 mmol, 1 eq) and 1-ethyl-3,5-dimethyl-1H-pyrazole-4-carbaldehyde (207 mg, 1.36 mmol, 1.5 eq) in tetrahydrofuran (10 mL) add sodium triacetoxyborohydride (480 mg, 2.26 mmol, 2.5 eq) in one portion as a solid. Stir the mixture at room temperature under nitrogen for 19 hr. Add 2M aqueous sodium hydroxide solution (10 ml) and DCM (20 ml) separate and extract the aqueous layer with DCM (20 ml). Combine the organics, dry over magnesium sulfate, filter and concentrate. Purify by high pH reverse phase HPLC. Dissolve this material (49 mg, 0.12 mmol), in the minimum quantity of 50% aqueous acetonitrile. Add 2M aqueous hydrogen chloride (60 μL, 0.12 mmol) and lyophilize to give the title compound (58 mg, 15%). MS (ES): m/z=395.2 [M+H]+.

후처리

  1. customseparate
  2. extractionextract the aqueous layer with DCM (20 ml)
  3. dry with materialCombine the organics, dry over magnesium sulfate
  4. filtrationfilter
  5. concentrationconcentrate
  6. customPurify by high pH reverse phase HPLC

출처 및 근거

ORD 기록
ord-b8e8b01beb84434e9f3da647114b4aad
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202873B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트