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Hydrochloric Acid → HCID 86748258, 화합물

HRID 2380098
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HRID 2380098 반응식
C(O[C:6]([NH:8][C@H:9]([C@H:14]1[O:18][C:17](=[O:19])[C@H:16]([C:20]([OH:23])([CH3:22])[CH3:21])[CH2:15]1)[CH2:10][CH:11]([CH3:13])[CH3:12])=[O:7])(C)(C)C.Cl.[C:25]([O:29][C:30]([NH:32][C@H:33](C(O)=O)[CH2:34][C:35]1[N:36]=[CH:37][S:38][CH:39]=1)=[O:31])([CH3:28])([CH3:27])[CH3:26].P([C:51]#[N:52])(OCC)(OCC)=O.C(N([CH2:58][CH3:59])CC)C.O1CCO[CH2:62][CH2:61]1>>[C:25]([O:29][C:30]([NH:32][C@H:33]([C:6]([NH:8][C@@H:9]([CH2:10][CH:11]([CH3:12])[CH3:13])[C@@H:14]([OH:18])[CH2:15][C@@H:16]([C:20]([OH:23])([CH3:21])[CH3:22])[C:17]([NH:52][CH2:51][CH:58]([CH3:59])[CH2:61][CH3:62])=[O:19])=[O:7])[CH2:34][C:35]1[N:36]=[CH:37][S:38][CH:39]=1)=[O:31])([CH3:26])([CH3:27])[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 6

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 312751,4-DioxaneHCID 76257Diethyl cyanophosphonateHCID 2734486(S)-2-((tert-Butoxycarbonyl)amino)-3-(thiazol-4-yl)propanoic acidHCID 14483174HCID 14483174, 화합물

생성물 1

HCID 86748258
HCID 86748258, 화합물
수율 85%

실험 절차

Following a procedure similar to that described in Example 1, a mixture of 260 mg (0.62 mmoles) of (3S, 5S)-5-[(1S)-1-(N-t-butoxycarbonylamino)-3-methylbutyl]-3-(1-hydroxy-1-methylethyl)dihydrofuran-2(3H)-one (prepared as described in Preparation 9) in 5 ml of a 4N solution of hydrogen chloride in dioxane was stirred at room temperature for 30 minutes. At the end of this time, the solvent was removed by distillation under reduced pressure, and diethyl ether was added to the residue. The solvent was then again removed by distillation under reduced pressure. This operation was repeated in total three times, after which the residue was dried under vacuum for 8 hours. At the end of this time, the dried material was suspended in 5 ml of anhydrous tetrahydrofuran, and 187 mg (0.69 mmoles) of N-(t-butoxycarbonyl)-3-(4-thiazolyl)-L-alanine were added to the resulting suspension, followed by 0.11 ml (0.73 mmoles) of 95% diethyl cyanophosphate and 0.19 ml (1.36 mmoles) of triethylamine, all whilst ice-cooling and under an atmosphere of nitrogen. The mixture was then stirred for 6 hours, after which the solvent was removed by distillation under reduced pressure, and the residue was purified by medium pressure silica gel column chromatography (using a 20:1 by volume mixture of methylene chloride and methanol as eluent), to give 303 mg (yield 85%) of the title compound as an amorphous substance.

후처리

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure, and diethyl ether
  2. additionwas added to the residue
  3. customThe solvent was then again removed by distillation under reduced pressure
  4. customafter which the residue was dried under vacuum for 8 hours
  5. temperatureall whilst ice-cooling and under an atmosphere of nitrogen
  6. stirringThe mixture was then stirred for 6 hours
  7. customafter which the solvent was removed by distillation under reduced pressure
  8. customthe residue was purified by medium pressure silica gel column chromatography (
  9. additionby volume mixture of methylene chloride and methanol as eluent),

출처 및 근거

ORD 기록
ord-02fd7291ff9d4875ba6e88233c1eb96d
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364844

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