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

Potassium Carbonate → HCID 59627213, 화합물

HRID 1523254
노트
인쇄 미리보기

반응식

HRID 1523254 반응식
CS(O[CH2:6][CH2:7][CH2:8][C@:9]1([C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)[CH2:14][CH2:13][N:12]([C@H:15]([C:17]2[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=2)[CH3:16])[C:11](=[O:24])[NH:10]1)(=O)=O.[CH3:32][S:33]([NH2:36])(=[O:35])=[O:34].C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[Br:23][C:20]1[CH:21]=[CH:22][C:17]([C@@H:15]([N:12]2[CH2:13][CH2:14][C@:9]([CH2:8][CH2:7][CH2:6][NH:36][S:33]([CH3:32])(=[O:35])=[O:34])([C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)[NH:10][C:11]2=[O:24])[CH3:16])=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 72879MethanesulfonamideHCID 59627236HCID 59627236, 화합물

생성물 1

HCID 59627213HCID 59627213, 화합물수율 14.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 3-((R)-1-((S)-1-(4-bromophenyl)ethyl)-4-(4-fluorophenyl)-2-oxohexa hydropyrimidin-4-yl)propyl methanesulfonate (58 mg, 0.11 mmol) and methanesulfonamide (105 mg, 1.10 mmol) in acetone (10 mL) was added K2CO3 (31 mg, 0.22 mmol), and the mixture was refluxed overnight. The reaction was quenched with water, and the mixture was extracted with EtOAc. After removal of the solvent, the mixture was extracted with EtOAc, and the organic solution was washed with brine, dried over Na2SO4, filtered and concentrated to give the crude product, which was purified by preparative TLC and preparative HPLC to give N-(3-((R)-1-((S)-1-(4-bromophenyl)ethyl)-4-(4-fluorophenyl)-2-oxohexahydropyrimidin-4-yl)propyl)methanesulfonamide (8 mg, 14%). 1H NMR (CDCl3): 1.18□m, 1H), 1.45 (d, 3H), 1.50 (m, 1H), 1.88-2.16 (m, 5H), 2.84 (m, 4H), 3.02 (m, 2H), 4.70 (s, 1H), 5.63 (m, 1H), 6.88-6.98 (m, 4H), 7.12 (m, 2H), 7.30 (m, 2H). LC-MS Method 1 tR=1.146 min, m/z=512.

후처리

  1. temperaturethe mixture was refluxed overnight
  2. customThe reaction was quenched with water
  3. extractionthe mixture was extracted with EtOAc
  4. customAfter removal of the solvent
  5. extractionthe mixture was extracted with EtOAc
  6. washthe organic solution was washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give the crude product, which
  11. customwas purified by preparative TLC and preparative HPLC

출처 및 근거

ORD 기록
ord-b5d88c1e3e674be3a4f555c5dcd923ae
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079861B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트