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Triethyl phosphonoacetate → HCID 67296271、化合物

HRID 2276834
ノート
印刷プレビュー

反応式

HRID 2276834 の反応式
[H-].[Na+].C(OP([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])(OCC)=O)C.[C:17]([O:21][C:22](=[O:49])[N:23]([C@H:36]1[CH2:40][CH2:39][C@@H:38]([C:41]2[CH:46]=[CH:45][C:44]([CH:47]=O)=[CH:43][CH:42]=2)[CH2:37]1)[C@@H:24]([C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=[CH:28][CH:27]=1)[CH3:25])([CH3:20])([CH3:19])[CH3:18].[Cl-].[NH4+]>O1CCCC1>[CH2:15]([O:14][C:12](=[O:13])/[CH:11]=[CH:47]/[C:44]1[CH:45]=[CH:46][C:41]([C@@H:38]2[CH2:39][CH2:40][C@H:36]([N:23]([C:22]([O:21][C:17]([CH3:18])([CH3:20])[CH3:19])=[O:49])[C@@H:24]([C:26]3[C:35]4[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=4)[CH:29]=[CH:28][CH:27]=3)[CH3:25])[CH2:37]2)=[CH:42][CH:43]=1)[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 86665256HCID 86665256、化合物

生成物 1

HCID 67296271HCID 67296271、化合物収率 100.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

Under a nitrogen stream, sodium hydride (60% in mineral-oil dispersion) (44 mg, 1.1 mmol) was suspended in tetrahydrofuran (5 mL), followed by addition of ethyl diethylphosphonoacetate (0.24 mL, 1.2 mmol), and the mixture was stirred for 10 minutes at room temperature. A tetrahydrofuran solution of [(1S,3R)-3-(4-formylphenyl)cyclopentyl][(1R)-1-(naphthalen-1-yl)ethyl]carbamic acid tert-butyl ester (407 mg, 0.92 mmol) was added to the mixture, and the mixture was stirred further for 1 hour at room temperature. A saturated aqueous ammonium chloride solution was added to the reaction solution, and the solution was extracted with ethyl acetate. The extracted solution was dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue obtained was purified by column chromatography (ethyl acetate/hexane: 10/90-15/85) to give the title compound (475 mg).

後処理

  1. stirringthe mixture was stirred further for 1 hour at room temperature
  2. extractionthe solution was extracted with ethyl acetate
  3. dry with materialThe extracted solution was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue obtained
  6. customwas purified by column chromatography (ethyl acetate/hexane: 10/90-15/85)

出典と根拠

ORDレコード
ord-0e188144259846cd96774925eca81a88
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133140B2

反応ノート

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