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Hydrochloric Acid → (2R, 4S, 5S)-5-{N-[2(R)-Benzyl-3-(morpholinocarbonyl)propionyl]-3-(4-thiazolyl)-L-alanyl}amino-6-cyclohexyl-4-hydroxy-2,N-dimethylhexanamide

HRID 1768834
ノート
印刷プレビュー

反応式

HRID 1768834 の反応式
C(O[C:6]([NH:8][C@H:9]([C:16]([NH:18][C@@H:19]([CH2:29][CH:30]1[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1)[C@@H:20]([OH:28])[CH2:21][C@@H:22]([CH3:27])[C:23]([NH:25][CH3:26])=[O:24])=[O:17])[CH2:10][C:11]1[N:12]=[CH:13][S:14][CH:15]=1)=[O:7])(C)(C)C.Cl.[CH2:37]([C@H:44]([CH2:48][C:49]([N:51]1[CH2:56][CH2:55][O:54][CH2:53][CH2:52]1)=[O:50])C(O)=O)[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1.C(P(=O)(OCC)OCC)#N.C(N(CC)CC)C>O1CCOCC1.CO>[CH2:37]([C@H:44]([CH2:48][C:49]([N:51]1[CH2:52][CH2:53][O:54][CH2:55][CH2:56]1)=[O:50])[C:6]([NH:8][C@H:9]([C:16]([NH:18][C@@H:19]([CH2:29][CH:30]1[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]1)[C@@H:20]([OH:28])[CH2:21][C@@H:22]([CH3:27])[C:23]([NH:25][CH3:26])=[O:24])=[O:17])[CH2:10][C:11]1[N:12]=[CH:13][S:14][CH:15]=1)=[O:7])[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 142130822(R)-benzyl-3-(morpholinocarbonyl)propionic acidHCID 15045762(2R, 4S, 5S)-5-[N-(t-Butoxycarbonyl)-3-(4-thiazolyl)-L-alanyl]amino-6-cyclohexyl-4-hydroxy-2, N-dimethylhexanamide

生成物 1

HCID 15045748
(2R, 4S, 5S)-5-{N-[2(R)-Benzyl-3-(morpholinocarbonyl)propionyl]-3-(4-thiazolyl)-L-alanyl}amino-6-cyclohexyl-4-hydroxy-2,N-dimethylhexanamide
収率 34.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 110 mg (0.215 mmole) of (2R, 4S, 5S)-5-[N-(t-butoxycarbonyl)-3-(4-thiazolyl)-L-alanyl]amino-6-cyclohexyl-4-hydroxy-2,N-dimethylhexanamide [prepared as described in step (a) above], 2 ml of methanol and 2 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. The residue was mixed with benzene and the solvent was stripped from the mixture by distillation under reduced pressure. After this operation had been repeated three times, the final residue was dried in vacuo for 8 hours. The dried material was then suspended in 8 ml of anhydrous tetrahydrofuran, and 59.6 mg (0.215 mmole) of 2(R)-benzyl-3-(morpholinocarbonyl)propionic acid were added to the suspension. 0.042 ml (0.258 mmole) of 95% diethyl cyanophosphonate and 0.12 ml (0.86 mmole) of triethylamine were then added to the mixture, and the resulting mixture was stirred for 18 hours. At the end of this time, the reaction mixture was concentrated by distillation under reduced pressure, and the residue was purified by preparative thin layer chromatography on silica gel (using a 10:1 by volume mixture of methylene chloride and methanol as the developing solvent), to afford 50 mg of the title compound as a white powder.

後処理

  1. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  2. additionThe residue was mixed with benzene
  3. distillationthe solvent was stripped from the mixture by distillation under reduced pressure
  4. dry with materialthe final residue was dried in vacuo for 8 hours
  5. stirringthe resulting mixture was stirred for 18 hours
  6. concentrationAt the end of this time, the reaction mixture was concentrated by distillation under reduced pressure
  7. customthe residue was purified by preparative thin layer chromatography on silica gel (
  8. additionby volume mixture of methylene chloride and methanol as the developing solvent),

出典と根拠

ORDレコード
ord-795208f94bb44a038e281f7d5b2f8e07
出典データセット
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05378689

反応ノート

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