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Hydrochloric Acid → HCID 14989069, 화합물

HRID 2380099
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HRID 2380099 반응식
C(OC(N[C@H:9]([C:16]([NH:18][C@@H:19]([CH2:36][CH:37]([CH3:39])[CH3:38])[C@@H:20]([OH:35])[CH2:21][C@@H:22]([C:31]([OH:34])([CH3:33])[CH3:32])[C:23]([NH:25][CH2:26][CH:27]([CH3:30])CC)=[O:24])=[O:17])[CH2:10][C:11]1[N:12]=[CH:13][S:14][CH:15]=1)=O)(C)(C)C.Cl.[C:41]([O:45][C:46]([NH:48][C@H:49]([C:61](O)=[O:62])[CH2:50][C:51]1[C:60]2[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=2)[CH:54]=[CH:53][CH:52]=1)=[O:47])([CH3:44])([CH3:43])[CH3:42].P(C#N)(OCC)(O[CH2:67][CH3:68])=O.C([N:76](CC)CC)C>O1CCOCC1>[C:41]([O:45][C:46]([NH:48][C@H:49]([C:61]([NH:76][C@H:9]([C:16]([NH:18][C@@H:19]([CH2:36][CH:37]([CH3:39])[CH3:38])[C@@H:20]([OH:35])[CH2:21][C@@H:22]([C:31]([OH:34])([CH3:33])[CH3:32])[C:23]([NH:25][CH2:26][CH:27]([CH3:30])[CH2:67][CH3:68])=[O:24])=[O:17])[CH2:10][C:11]1[N:12]=[CH:13][S:14][CH:15]=1)=[O:62])[CH2:50][C:51]1[C:60]2[C:55](=[CH:56][CH:57]=[CH:58][CH:59]=2)[CH:54]=[CH:53][CH:52]=1)=[O:47])([CH3:42])([CH3:44])[CH3:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 7021841Boc-3-(1-naphthyl)-L-alanineHCID 86748258HCID 86748258, 화합물

생성물 1

HCID 14989069HCID 14989069, 화합물수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 142 mg (0.25 mmoles) of (2S, 4S, 5S)-5-{N-[N-(t-butoxycarbonyl)-3-(4-thiazolyl)-L-alanyl]}amino-4-hydroxy-2-(1-hydroxy-1-methylethyl)-7-methyl-N-[2(RS)-methylbutyl]octanamide (prepared as described in Example 6) 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. Diethyl ether was then added to the residue, and the solvent was removed again 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 10 ml of anhydrous tetrahydrofuran, and 99.9 mg (0.32 mmoles) of N-t-butoxycarbonyl-3-(1 naphthyl)-L-alanine were added to the resulting suspension, followed by 0.05 ml (0.33 mmoles) of 95% diethyl cyanophosphate and 0.12 ml (0.86 mmoles) of triethylamine, all whilst ice-cooling and under an atmosphere of nitrogen, The mixture was then stirred for 8 hours, after which the solvent was removed by distillation under reduced pressure, and the residue was purified by silica gel thin layer chromatography (using a 10:1 by volume mixture of methylene chloride and methanol as developing solvent), to give 181 mg (yield 95%) of the title compound as white crystals, melting at 90°-92° C.

후처리

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. additionDiethyl ether was then added to the residue
  3. customthe solvent was removed again 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 8 hours
  7. customafter which the solvent was removed by distillation under reduced pressure
  8. customthe residue was purified by silica gel thin layer chromatography (
  9. additionby volume mixture of methylene chloride and methanol as developing solvent),

출처 및 근거

ORD 기록
ord-5838f0dbd76a49119202cbcbfa847a58
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05364844

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