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

Triethylamine → 1-{4-[2-(2-Aminopyrimidin-5-yl)-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-8-yl]-cis-2,6-dimethylpiperazin-1-yl}-1-oxopropan-2-ol

HRID 1876615
노트
인쇄 미리보기

반응식

HRID 1876615 반응식
C(N(CC)CC)C.C([O:11][C@@H:12]([CH3:16])[C:13](Cl)=[O:14])(=O)C.[CH3:17][C@H:18]1[NH:23][C@@H:22]([CH3:24])[CH2:21][N:20]([C:25]2[N:26]([CH2:47][C:48]([F:51])([F:50])[F:49])[C:27]3[C:32]([N:33]=2)=[C:31]([N:34]2[CH2:39][CH2:38][O:37][CH2:36][CH2:35]2)[N:30]=[C:29]([C:40]2[CH:41]=[N:42][C:43]([NH2:46])=[N:44][CH:45]=2)[N:28]=3)[CH2:19]1.C[O-].[Na+].CO>C(Cl)Cl.CO.C(Cl)Cl.CO>[NH2:46][C:43]1[N:44]=[CH:45][C:40]([C:29]2[N:28]=[C:27]3[C:32]([N:33]=[C:25]([N:20]4[CH2:21][C@@H:22]([CH3:24])[N:23]([C:13](=[O:14])[CH:12]([OH:11])[CH3:16])[C@@H:18]([CH3:17])[CH2:19]4)[N:26]3[CH2:47][C:48]([F:50])([F:49])[F:51])=[C:31]([N:34]3[CH2:35][CH2:36][O:37][CH2:38][CH2:39]3)[N:30]=2)=[CH:41][N:42]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471Triethylamine2회HCID 11094804(1S)-2-Chloro-1-methyl-2-oxoethyl acetate3회HCID 23694274Sodium methanolate methanolHCID 453780145-[8-(cis-3,5-dimethylpiperazin-1-yl)-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl]pyrimidin-2-amine

생성물 1

HCID 59333616
1-{4-[2-(2-Aminopyrimidin-5-yl)-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-8-yl]-cis-2,6-dimethylpiperazin-1-yl}-1-oxopropan-2-ol
수율 102.1%

시약·촉매·용매 3

HCID 887Methanol용매HCID 6344Dichloromethane용매2회HCID 21226129Dichloromethane methanol용매2회

실험 절차

Triethylamine (70.2 μl, 0.50 mmol) and (S)-(−)-2-acetoxypropionyl chloride (32.9 μl, 0.25 mmol) were added to a methylene chloride suspension (7.0 ml) of 5-[8-(cis-3,5-dimethylpiperazin-1-yl)-6-morpholin-4-yl-9-(2,2,2-trifluoroethyl)-9H-purin-2-yl]pyrimidin-2-amine (112.7 mg, 0.23 mmol) with ice cooling. The resulting mixture was stirred at room temperature for 3 hours followed by the addition of (S)-(−)-2-acetoxypropionyl chloride (9.0 μl, 0.07 mmol) with ice cooling and the resulting mixture was stirred at room temperature for 1 day. The reaction mixture was poured into methylene chloride-methanol (10:1), washed with saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, the resulting residue was dissolved in methylene chloride (7.0 ml) followed by the addition of triethylamine (140.3 μl, 1.01 mmol) and (S)-(−)-2-acetoxypropionyl chloride (65.7 μl, 0.50 mmol) with ice cooling, and the resulting mixture was stirred at room temperature for 1 day. The reaction mixture was poured into methylene chloride-methanol (10:1), washed with saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, a 25% by weight sodium methoxide-methanol solution (157.0 μl, 0.69 mmol) was added to a methanol (6.0 ml) solution of the resulting residue, and the resulting mixture was stirred at 50° C. for 22 hours. The resulting mixture was left standing to cool and then the reaction mixture was poured into methylene chloride and washed with saturated brine. The organic layer was dried over anhydrous sodium sulfate, the mixture was filtrated, the filtrate was concentrated under reduced pressure, and the resulting residue was purified by preparative thin layer silica gel chromatography (methylene chloride:methanol=10:1) to give the title compound (132.6 mg, 96%) as a pale yellow solid.

후처리

  1. stirringthe resulting mixture was stirred at room temperature for 1 day
  2. washwashed with saturated aqueous sodium hydrogen carbonate solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationAfter filtration
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. dissolutionthe resulting residue was dissolved in methylene chloride (7.0 ml)
  7. stirringthe resulting mixture was stirred at room temperature for 1 day
  8. washwashed with saturated aqueous sodium hydrogen carbonate solution
  9. dry with materialdried over anhydrous sodium sulfate
  10. filtrationAfter filtration
  11. concentrationthe filtrate was concentrated under reduced pressure
  12. stirringthe resulting mixture was stirred at 50° C. for 22 hours
  13. waitThe resulting mixture was left
  14. temperatureto cool
  15. washwashed with saturated brine
  16. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  17. filtrationthe mixture was filtrated
  18. concentrationthe filtrate was concentrated under reduced pressure
  19. customthe resulting residue was purified by preparative thin layer silica gel chromatography (methylene chloride:methanol=10:1)

출처 및 근거

ORD 기록
ord-a9f3c9992ca74ac0abf8b3f2a2695778
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309546B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트