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Ammonium Acetate → HCID 178502297, 화합물

HRID 535124
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HRID 535124 반응식
[CH3:1][O:2][C:3](=[O:62])[NH:4][C@H:5]([C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C@H:12]1[C:16]1[NH:17][CH:18]=[C:19]([C:21]2[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][C:30]([C:33](=O)[CH2:34][NH:35][C:36]([CH:38]4[CH2:42][C:41]5([CH2:47][CH2:46][S:45](=[O:49])(=[O:48])[CH2:44][CH2:43]5)[CH2:40][N:39]4[C:50](=[O:60])[C@@H:51]([NH:55][C:56]([O:58][CH3:59])=[O:57])[CH:52]([CH3:54])[CH3:53])=O)=[CH:29][CH:28]=3)=[CH:23][CH:22]=2)[N:20]=1)=[O:10])[CH:6]([CH3:8])[CH3:7].C([O-])(=O)C.[NH4+:67]>O1CCOCC1.C(OCC)(=O)C>[CH3:7][CH:6]([CH3:8])[C@H:5]([NH:4][C:3](=[O:62])[O:2][CH3:1])[C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C@H:12]1[C:16]1[NH:17][CH:18]=[C:19]([C:21]2[CH:22]=[CH:23][C:24]([C:27]3[CH:28]=[CH:29][C:30]([C:33]4[N:67]=[C:36]([CH:38]5[CH2:42][C:41]6([CH2:43][CH2:44][S:45](=[O:49])(=[O:48])[CH2:46][CH2:47]6)[CH2:40][N:39]5[C:50](=[O:60])[C@@H:51]([NH:55][C:56]([O:58][CH3:59])=[O:57])[CH:52]([CH3:53])[CH3:54])[NH:35][CH:34]=4)=[CH:31][CH:32]=3)=[CH:25][CH:26]=2)[N:20]=1)=[O:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 517165Ammonium AcetateHCID 178502298HCID 178502298, 화합물

생성물 1

HCID 178502297HCID 178502297, 화합물수율 37.9%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

반응 조건

온도
110 °C

실험 절차

A solution of methyl((1S)-2-methyl-1-{[(2S)-2-(4-{4′-[({[2-((2S)-3-methyl-2-{[(methyloxy)carbonyl]amino}butanoyl)-8,8-dioxido-8-thia-2-azaspiro[4.5]dec-3-yl]carbonyl}amino)acetyl]-4-biphenylyl}-1H-imidazol-2-yl)-1-pyrrolidinyl]carbonyl}propyl)carbamate (108) (107 mg, 0.12 mmol) and ammonium acetate (94 mg, 1.2 mmol) in dioxane (1.5 mL) was degassed with nitrogen and heated to 110° C. in a sealed tube for 18 h. The reaction was cooled to room temperature and diluted with ethyl acetate and filtered and concentrated in vacuo. Purified by SFC to afford the product as a tan solid (39 mg, 37% yield). 1H NMR (400 MHz, METHANOL-d4) δ ppm 7.64 (br. s., 10H) 7.32 (br. s., 2H) 5.05-5.24 (m, 1H) 4.04-4.29 (m, 1H) 3.99 (br. s., 1H) 3.81 (br. s., 1H) 3.55-3.73 (m, 6H) 3.03-3.25 (m, 4H) 1.80-2.47 (m, 14H) 0.68-1.06 (m, 16H). HRMS for C44H57N8O8S (M+H)+ calc: 857.4020. found: 857.4020. Purity (LC-MS): 97%.

후처리

  1. temperatureThe reaction was cooled to room temperature
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customPurified by SFC

출처 및 근거

ORD 기록
ord-fbc1b6f374514c9cac1c568c91f11d52
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853416B2

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