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Hydrochloric Acid → HCID 14989069、化合物

HRID 2380099
ノート
印刷プレビュー

反応式

HRID 2380099 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

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

生成物 1

HCID 14989069HCID 14989069、化合物収率 95%

試薬・触媒・溶媒

1
HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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),

出典と根拠

ORDレコード
ord-5838f0dbd76a49119202cbcbfa847a58
出典データセット
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05364844

反応ノート

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