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Lithium Hydroxide → (RS)-N-(4-cyano-benzyl)-2-ethoxy-malonamic acid

HRID 1828115
ノート
印刷プレビュー

反応式

HRID 1828115 の反応式
C([O:3][C:4](=[O:21])[CH:5]([O:18][CH2:19][CH3:20])[C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]#[N:17])=[CH:12][CH:11]=1)=[O:7])C.[Li+].[OH-]>CO.O.C1COCC1>[C:16]([C:13]1[CH:12]=[CH:11][C:10]([CH2:9][NH:8][C:6](=[O:7])[CH:5]([O:18][CH2:19][CH3:20])[C:4]([OH:21])=[O:3])=[CH:15][CH:14]=1)#[N:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 3939Lithium HydroxideHCID 69641469HCID 69641469、化合物

生成物 1

HCID 22064699(RS)-N-(4-cyano-benzyl)-2-ethoxy-malonamic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A mixture of (RS)-N-(4-cyano-benzyl)-2-ethoxy-malonamic acid ethyl ester (1.97 g) and LiOH (285 mg) in MeOH (14 ml), H2O (7 ml) and THF (14 ml) was stirred 3 h at 60° C. The solvents were evaporated, EtOAc was added and it was washed with HCl 0.1 N, water and brine. The aqueous phases were extracted again with more EtOAc. The combined organic phases were dried (MgSO4) and the solvent was removed to yield (RS)-N-(4-cyano-benzyl)-2-ethoxy-malonamic acid, 1.53 g (86%); of white solid. MS 260.2 (100, [M+H]+), 277.2 (13, [M+NH4]+)

後処理

  1. customThe solvents were evaporated
  2. additionEtOAc was added
  3. washit was washed with HCl 0.1 N, water and brine
  4. extractionThe aqueous phases were extracted again with more EtOAc
  5. dry with materialThe combined organic phases were dried (MgSO4)
  6. customthe solvent was removed

出典と根拠

ORDレコード
ord-98a9eab62cf548129def9128896d146b
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07056932B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート