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

Hydrochloric Acid → HCID 67682542, 화합물

HRID 1751590
노트
인쇄 미리보기

반응식

HRID 1751590 반응식
[CH3:1][C:2]1([CH3:32])[C:6]([CH3:8])([CH3:7])[O:5][B:4]([C:9]2[CH:10]=[CH:11][C:12]3[N:16]=[C:15]([C@@H:17]4[C@@H:22]5[CH2:23][C@@H:19]([CH2:20][CH2:21]5)[N:18]4C(OC(C)(C)C)=O)[NH:14][C:13]=3[CH:31]=2)[O:3]1.Cl.O1CCOCC1.[CH3:40][O:41][C:42]([NH:44][C@@H:45]([CH:49]([CH3:51])[CH3:50])[C:46](O)=[O:47])=[O:43].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C>C(OCC)(=O)C.CO>[CH3:50][CH:49]([CH3:51])[C@H:45]([NH:44][C:42](=[O:43])[O:41][CH3:40])[C:46](=[O:47])[N:18]1[C@H:17]([C:15]2[NH:14][C:13]3[CH:31]=[C:9]([B:4]4[O:5][C:6]([CH3:8])([CH3:7])[C:2]([CH3:32])([CH3:1])[O:3]4)[CH:10]=[CH:11][C:12]=3[N:16]=2)[C@@H:22]2[CH2:23][C@H:19]1[CH2:20][CH2:21]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 10942966(2S)-2-((methoxycarbonyl)amino)-3-methylbutanoic acid
HCID 67506198
(1R,3S,4S)-tert-butyl 3-(6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-benzo[d]imidazol-2-yl)-2-azabicyclo[2.2.1]heptane-2-carboxylate

생성물 1

HCID 67682542HCID 67682542, 화합물수율 95%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of (1R,3S,4S)-tert-butyl 3-(6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-benzo[d]imidazol-2-yl)-2-azabicyclo[2.2.1]heptane-2-carboxylate (1.0 g, 2.3 mmol), methanol (10 mL), and 4M HCl in dioxane (11 mL, 44 mmol) was stirred at room temperature. The reaction was thoroughly concentrated after one hour. The resulting residue was dissolved in dimethylformamide (11.4 mL). To this solution was added (S)-2-(methoxycarbonylamino)-3-methylbutanoic acid (419 mg, 2.4 mmol) and HATU (909 mg, 2.4 mmol). Diisopropylethylamine (1.4 mL, 8.1 mmol) was added and the reaction was stirred at room temperature. After thirty minutes, the reaction was diluted with ethyl acetate. The organic phase was washed with water and brine, dried (Na2SO4) and concentrated. The crude material was purified by flash column chromatography to yield methyl (S)-3-methyl-1-oxo-1-((1R,3S,4S)-3-(6-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-benzo[d]imidazol-2-yl)-2-azabicyclo[2.2.1]heptan-2-yl)butan-2-ylcarbamate (1.08 g, 95%).

후처리

  1. concentrationThe reaction was thoroughly concentrated after one hour
  2. dissolutionThe resulting residue was dissolved in dimethylformamide (11.4 mL)
  3. waitAfter thirty minutes
  4. washThe organic phase was washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customThe crude material was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-200df816b9cc4cc6ad19be0895bed063
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156823B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트