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盐酸 → HCID 86748258,化合物

HRID 2380098
笔记
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反应方程式

HRID 2380098 反应方程式
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]
参与物实验过程后处理来源与证据反应笔记

参与物

7

反应物 6

HCID 313盐酸HCID 8471三乙胺HCID 312751,4-二氧六环HCID 76257氰基磷酸二乙酯HCID 2734486(S)-2-((tert-Butoxycarbonyl)amino)-3-(thiazol-4-yl)propanoic acidHCID 14483174HCID 14483174,化合物

产物 1

HCID 86748258
HCID 86748258,化合物
收率 85%

实验过程

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.

后处理

  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),

来源与证据

ORD记录
ord-02fd7291ff9d4875ba6e88233c1eb96d
来源数据集
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
专利号
US05364844

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记