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

1,2-Dimethoxyethane → (1R,6S)-tert-butyl 8-(4-(dimethylamino)pyridin-2-yl)-3,8-diazabicyclo[4.2.0]octane-3-carboxylate

HRID 1193096
노트
인쇄 미리보기

반응식

HRID 1193096 반응식
C[C:2]1[N:7]=[C:6]([N:8]2[C@@H:15]3[C@@H:10]([CH2:11][CH2:12][NH:13][CH2:14]3)[CH2:9]2)[CH:5]=[CH:4][CH:3]=1.ClC1C=C([N:23]([CH3:25])[CH3:24])C=CN=1.[CH3:26][C:27]([CH3:30])([O-:29])[CH3:28].[K+].[CH3:32][O:33]CCOC>O>[CH3:25][N:23]([CH3:24])[C:4]1[CH:3]=[CH:2][N:7]=[C:6]([N:8]2[C@@H:15]3[C@@H:10]([CH2:11][CH2:12][N:13]([C:32]([O:29][C:27]([CH3:30])([CH3:28])[CH3:26])=[O:33])[CH2:14]3)[CH2:9]2)[CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 80711,2-DimethoxyethaneHCID 109864952-Chloro-4-(dimethylamino)pyridineHCID 23665647Potassium tert-butoxideHCID 67116915(1R,6S)-8-(6-Methylpyridin-2-yl)-3,8-diazabicyclo[4.2.0]octane

생성물 1

HCID 67117087(1R,6S)-tert-butyl 8-(4-(dimethylamino)pyridin-2-yl)-3,8-diazabicyclo[4.2.0]octane-3-carboxylate수율 52%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

To a microwave safe vial was added Intermediate 40 (200 mg, 0.94 mmol), 2-chloro-N,N-dimethylpyridin-4-amine (134 mg, 0.85 mmol), chloro[(1,2,3-n)-3-phenyl-2-propenyl][1,3-bis(2,6-di-1-propylphenyl)-4,5-dihydroimidazol-2-ylidene]palladium(II) (5.6 mg, 0.0086 mmol), potassium tert-butoxide (96.1 mg, 0.85 mmol) and DME (8 mL). The resulting mixture was heated to 100° C. After 1 hour the mixture was allowed to cool to ambient temperature at which time water (20 mL) was added. The aqueous layer was extracted with DCM (15 mL) three times. The organic layers were combined, dried over Na2SO4, filtered, and concentrated under reduced pressure. The crude residue was purified by reverse-phase HPLC (basic) to yield (1R,6S)-tert-butyl 8-(4-(dimethylamino)pyridin-2-yl)-3,8-diazabicyclo[4.2.0]octane-3-carboxylate (150 mg, 52%). MS (ESI) mass calcd. for C18H28N4O2, 332.2; m/z found, 333.2 [M+H]+. 1H NMR (500 MHz, CDCl3): 7.84 (d, J=5.7 Hz, 1H), 6.02 (d, J=5.6 Hz, 1H), 5.45-5.31 (m, 1H), 4.47-4.35 (m, 1H), 4.09-3.96 (m, 1H), 3.91 (t, J=7.7 Hz, 1H), 3.86-3.72 (m, 2H), 3.55-3.26 (m, 2H), 2.95 (s, 6H), 2.85-2.70 (m, 1H), 2.06-1.95 (m, 1H), 1.90-1.84 (m, 1H), 1.45-1.29 (m, J=52.5 Hz, 9H).

후처리

  1. additionwas added
  2. extractionThe aqueous layer was extracted with DCM (15 mL) three times
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was purified by reverse-phase HPLC (basic)

출처 및 근거

ORD 기록
ord-4f0d8f5c41c64ef89390c426fea6d741
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680275B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트