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Hydrochloric Acid → HCID 86679524, 화합물

HRID 1776568
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HRID 1776568 반응식
[C:1]([S:4][C:5]([CH3:45])([CH3:44])[CH:6]([NH:36]C(OC(C)(C)C)=O)[C:7]([O:9][C@H:10]([C:21]1[CH:26]=[CH:25][C:24]([O:27][CH:28]([F:30])[F:29])=[C:23]([O:31][CH2:32][CH:33]2[CH2:35][CH2:34]2)[CH:22]=1)[CH2:11][C:12]1[C:17]([Cl:18])=[CH:16][N+:15]([O-:19])=[CH:14][C:13]=1[Cl:20])=[O:8])(=[O:3])[CH3:2].Cl.O1CCOCC1>C(Cl)Cl>[C:1]([S:4][C:5]([CH3:45])([CH3:44])[CH:6]([NH2:36])[C:7]([O:9][C@H:10]([C:21]1[CH:26]=[CH:25][C:24]([O:27][CH:28]([F:30])[F:29])=[C:23]([O:31][CH2:32][CH:33]2[CH2:35][CH2:34]2)[CH:22]=1)[CH2:11][C:12]1[C:13]([Cl:20])=[CH:14][N+:15]([O-:19])=[CH:16][C:17]=1[Cl:18])=[O:8])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 86679523HCID 86679523, 화합물

생성물 1

HCID 86679524HCID 86679524, 화합물수율 100.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4-((2S)-2-(3-(acetylthio)-2-(tert-butoxycarbonylamino)-3-methylbutanoyloxy)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)ethyl)-3,5-dichloropyridine 1-oxide (118 mg, 0.170 mmol) was dissolved in DCM (1 ml). HCl 4N in dioxane (425 μl, 1.70 mmol) was added and the mixture stirred for 30 minutes at RT. The reaction mixture was diluted with DCM. The organic layer was washed with NaHCO3 sat. sol. (2×) and brine, dried over Na2SO4 and evaporated under vacuum. The crude product was purified by preparative reverse-phase HPLC to give 101 mg of the desired compound (quantitative yield).

후처리

  1. washThe organic layer was washed with NaHCO3 sat. sol. (2×) and brine
  2. dry with materialdried over Na2SO4
  3. customevaporated under vacuum
  4. customThe crude product was purified by preparative reverse-phase HPLC

출처 및 근거

ORD 기록
ord-4294ce39af424e1484cf65c0105eeecd
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09265768B2

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