Ethoxalyl chloride → HCID 86691687、化合物

HRID 1407049ノート

反応式

HRID 1407049 の反応式
CCN(C(C)C)C(C)C.[NH2:10][CH2:11][CH:12]1[CH2:16][CH2:15][CH2:14][CH:13]1[NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21].Cl[C:26](=[O:32])[C:27]([O:29][CH2:30][CH3:31])=[O:28]>C1COCC1>[C:20]([O:19][C:18]([NH:17][CH:13]1[CH2:14][CH2:15][CH2:16][CH:12]1[CH2:11][NH:10][C:26](=[O:32])[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[O:24])([CH3:21])([CH3:23])[CH3:22]

参加物

5

反応物 3

HCID 20884Ethoxalyl chlorideHCID 81531DiisopropylethylamineHCID 53486461tert-Butyl [2-(aminomethyl)cyclopentyl]carbamate

生成物 1

HCID 86691687HCID 86691687、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

iPr2NEt (0.5 mL) was added into a solution of tert-butyl (2-(aminomethyl)cyclopentyl)carbamate (300 mg) and ethyl 2-chloro-2-oxoacetate (191 mg) in THF (10 mL). The reaction was stirred at room temperature for 16 hours before being quenched by water. The aqueous layer was extracted with EtOAc (3×20 mL). The combined organic phase was dried over MgSO4 and concentrated under vacuum to give the crude ethyl 2-(((2-((tert-butoxycarbonyl)amino)cyclopentyl)methyl)amino)-2-oxoacetate which was used as was.

後処理

  1. custombefore being quenched by water
  2. extractionThe aqueous layer was extracted with EtOAc (3×20 mL)
  3. dry with materialThe combined organic phase was dried over MgSO4
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-d67f042d66de46a68be52e5ec640668b
出典データセット
uspto-grants-2014_12
特許番号
US08916702B2

反応ノート

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