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

Hydrochloric Acid → 2-((S)-2-{(R)-4-[4-((R)-2,3-dihydroxy-propoxy)-phenyl]-2,5-dioxo-imidazolidin-1-yl}-3-phenyl-propionylamino)-thiazole-4-carboxylic acid methyl ester

HRID 2222981
노트
인쇄 미리보기

반응식

HRID 2222981 반응식
[CH3:1][O:2][C:3]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:45])[C@@H:12]([NH:20][C:21](=[O:44])[C@H:22]([NH2:43])[C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][C@H:31]([O:38][Si](C)(C)C)[CH2:32][O:33][Si](C)(C)C)=[CH:25][CH:24]=2)[CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[S:8][CH:9]=1)=[O:4].C(N(C(C)C)CC)(C)C.[O:55]=[C:56](Cl)OC(Cl)(Cl)Cl.Cl.C(=O)(O)[O-].[Na+]>ClCCl.C(OCC)(=O)C.O1CCCC1>[CH3:1][O:2][C:3]([C:5]1[N:6]=[C:7]([NH:10][C:11](=[O:45])[C@@H:12]([N:20]2[C:21](=[O:44])[C@@H:22]([C:23]3[CH:28]=[CH:27][C:26]([O:29][CH2:30][C@H:31]([OH:38])[CH2:32][OH:33])=[CH:25][CH:24]=3)[NH:43][C:56]2=[O:55])[CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[S:8][CH:9]=1)=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 10426DiphosgeneHCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 866040572-((S)-2-{(R)-2-amino-2-[4-((S)-2,3-bis-trimethylsilanyloxy-propoxy)-phenyl]-acetylamino}-3-phenyl-propionylamino)-thiazole-4-carboxylic acid methyl ester

생성물 1

HCID 58615468
2-((S)-2-{(R)-4-[4-((R)-2,3-dihydroxy-propoxy)-phenyl]-2,5-dioxo-imidazolidin-1-yl}-3-phenyl-propionylamino)-thiazole-4-carboxylic acid methyl ester
수율 52.6%

시약·촉매·용매 3

HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

반응 조건

온도
0 °C

실험 절차

2-((S)-2-{(R)-2-Amino-2-[4-((S)-2,3-bis-trimethylsilanyloxy-propoxy)-phenyl]-acetylamino}-3-phenyl-propionylamino)-thiazole-4-carboxylic acid methyl ester (100 mg, 0.15 mmol) and diisoproylethylamine (0.078 ml, 0.45 mmol) in dichloromethane (2 mL) were added to a solution of diphosgene (0.0143 ml, 0.12 mmol) in dichloromethane (2 mL) over 10 minute at 0° C. The mixture was stirred at 0° C. for 20 minute, diluted with ethyl acetate, washed with saturated sodium bicarbonate, brine and dried over sodium sulfate. Evaporation of solvents gave an oil which was dissolved in tetrahydrofuran (2 mL), treated with 1 N aqueous hydrochloric acid (0.45 ml, 0.45 mmol) and stirred for 3 hours. The reaction was neutralized with saturated aqueous sodium bicarbonate and extracted with ethyl acetate. The organic extracts were washed with brine and dried over magnesium sulfate. The crude product was purified by chromatography over silica gel gradient eluted with 100% ethyl acetate up to 3% v/v methanol in ethyl acetate to give 2-((S)-2-{(R)-4-[4-((R)-2,3-dihydroxy-propoxy)-phenyl]-2,5-dioxo-imidazolidin-1-yl}-3-phenyl-propionylamino)-thiazole-4-carboxylic acid methyl ester as a solid (35 mg, 42%).

후처리

  1. washwashed with saturated sodium bicarbonate, brine
  2. dry with materialdried over sodium sulfate
  3. customEvaporation of solvents
  4. customgave an oil which
  5. stirringstirred for 3 hours
  6. extractionextracted with ethyl acetate
  7. washThe organic extracts were washed with brine
  8. dry with materialdried over magnesium sulfate
  9. customThe crude product was purified by chromatography over silica gel gradient
  10. washeluted with 100% ethyl acetate up to 3% v/v methanol in ethyl acetate

출처 및 근거

ORD 기록
ord-11b9614a0a3547a79e84c1b3abebb4ee
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07371869B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트