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

Carbamate → (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide

HRID 1969636
노트
인쇄 미리보기

반응식

HRID 1969636 반응식
[C:1](=[O:4])([O-])[NH2:2].Cl.[CH3:6][C@@H:7]1[CH2:12][CH2:11][NH:10][CH2:9][C@@H:8]1[C:13]1[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1.CC[N:27]([CH:31](C)C)[CH:28]([CH3:30])C.C[C:35]#[N:36]>>[C:13]1([C@@H:8]2[C@H:7]([CH3:6])[CH2:12][CH2:11][N:10]([C:1]([NH:2][C:35]3[CH:30]=[CH:28][N:27]=[CH:31][N:36]=3)=[O:4])[CH2:9]2)[N:17]2[C:18]3[CH:24]=[CH:23][NH:22][C:19]=3[N:20]=[CH:21][C:16]2=[CH:15][N:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 276CarbamateHCID 6342Acetonitrile2회HCID 81531DiisopropylethylamineHCID 672171491-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride

생성물 1

HCID 67999614(3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide수율 9%

반응 조건

온도
70 °C

실험 절차

To solution of 4-aminopyrimidine (0.04 g, 0.43 mmol), TEA (0.07 mL, 0.47 mmol) and DMAP (0.006 g, 0.05 mmol), in MeCN (1 mL) at about 0° C. was added phenyl chloroformate (0.05 mL, 0.41 mmol). The reaction mixture was warmed to ambient temperature and stirred for about 3 h. To the reaction mixture was added water (2 mL) and Et2O (5 mL). The organic layer was separated, washed with water (2 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure to provide the crude carbamate. The carbamate was dissolved in MeCN (1 mL) and to it was added a solution of 1-((3R,4R)-4-methylpiperidin-3-yl)-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine hydrochloride (0.06 g, 0.21 mmol, Example #5 Step J) and DIEA (0.04 mL, 0.21 mmol) in MeCN (1 mL). The reaction mixture was heated to about 70° C. for about 2 h. The solvent was removed under reduced pressure. The crude residue was dissolved in DCM (5 mL) and washed with water (2 mL), brine (3 mL), dried over anhydrous MgSO4, filtered, and concd under reduced pressure. The crude material was purified by RP-HPLC (Table 1, Method e) to give (3R,4R)-3-(6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-1-yl)-4-methyl-N-(pyrimidin-4-yl)piperidine-1-carboxamide (0.007 g, 9%): LC/MS (Table 1, Method b) Rt=1.40 min; MS m/z 377 (M+H)+.

후처리

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe crude residue was dissolved in DCM (5 mL)
  3. washwashed with water (2 mL), brine (3 mL)
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customThe crude material was purified by RP-HPLC (Table 1, Method e)

출처 및 근거

ORD 기록
ord-2a68e081ac8d4703bec0577e598b2d6d
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426411B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트