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

Cesium carbonate → Racemic methyl-4-(5-{3-[(5-fluoro-4-methylpyrimidin-2-yl)amino]-5-methylphenyl}-1,3-thiazol-2-yl)-4-hydroxy-2,2-dimethylcyclohexanecarboxylate

HRID 410652
노트
인쇄 미리보기

반응식

HRID 410652 반응식
Cl[C:2]1[N:7]=[C:6]([CH3:8])[C:5]([F:9])=[CH:4][N:3]=1.[CH3:10][O:11][C:12]([CH:14]1[CH2:19][CH2:18][C:17]([C:21]2[S:22][C:23]([C:26]3[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]([NH2:33])[CH:27]=3)=[CH:24][N:25]=2)([OH:20])[CH2:16][C:15]1([CH3:35])[CH3:34])=[O:13].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C([O-])([O-])=O.[Cs+].[Cs+]>CC([O-])=O.CC([O-])=O.[Pd+2]>[CH3:10][O:11][C:12]([CH:14]1[CH2:19][CH2:18][C:17]([C:21]2[S:22][C:23]([C:26]3[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]([NH:33][C:2]4[N:7]=[C:6]([CH3:8])[C:5]([F:9])=[CH:4][N:3]=4)[CH:27]=3)=[CH:24][N:25]=2)([OH:20])[CH2:16][C:15]1([CH3:35])[CH3:34])=[O:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 207780732-Chloro-5-fluoro-4-methylpyrimidineHCID 67429727Methyl 4-(5-(3-amino-5-methylphenyl)thiazol-2-yl)-4-hydroxy-2,2-dimethylcyclohexanecarboxylate

생성물 1

HCID 67250082
Racemic methyl-4-(5-{3-[(5-fluoro-4-methylpyrimidin-2-yl)amino]-5-methylphenyl}-1,3-thiazol-2-yl)-4-hydroxy-2,2-dimethylcyclohexanecarboxylate
수율 86.5%

시약·촉매·용매 1

HCID 167845palladium(II) acetate촉매

반응 조건

온도
110 °C

실험 절차

Racemic 2-chloro-5-fluoro-4-methylpyrimidine (50.0 mg, 0.341 mmol), methyl-4-[5-(3-amino-5-methylphenyl)-1,3-thiazol-2-yl]-4-hydroxy-2,2-dimethylcyclohexanecarboxylate (128 mg, 0.341 mmol), Pd(OAc)2 (15.3 mg, 0.0680 mmol), Xantphos (59.2 mg, 0.102 mmol), and Cs2CO3 (222 mg, 0.682 mmol) were combined in a flask and degassed with argon. To this solid mixture was added dioxane (2.0 mL), and the resulting mixture was degassed with argon for 5 min. The reaction mixture was heated to 110° C. for 1.5 h. The reaction was cooled to ambient temperature, then diluted with saturated aqueous NaCl and EtOAc. The layers were separated, and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The resulting crude product was purified by column chromatography on silica (10-30% EtOAc/hexanes gradient) to afford racemic methyl-4-(5-{3-[(5-fluoro-4-methylpyrimidin-2-yl)amino]-5-methylphenyl}-1,3-thiazol-2-yl)-4-hydroxy-2,2-dimethylcyclohexanecarboxylate (143 mg, 0.295 mmol, 86% yield). MS ESI: [M+H]+ m/z 485.

후처리

  1. customdegassed with argon
  2. additionTo this solid mixture was added dioxane (2.0 mL)
  3. customthe resulting mixture was degassed with argon for 5 min
  4. temperatureThe reaction was cooled to ambient temperature
  5. additiondiluted with saturated aqueous NaCl and EtOAc
  6. customThe layers were separated
  7. extractionthe aqueous layer was extracted with EtOAc
  8. dry with materialThe combined organic layers were dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customThe resulting crude product was purified by column chromatography on silica (10-30% EtOAc/hexanes gradient)

출처 및 근거

ORD 기록
ord-13cbedf949f2436d80bbb8c6e77d72c1
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759366B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트