Lithium Hydroxide → Prt-062802

HRID 1944994ノート

反応式

HRID 1944994 の反応式
C1COCC1.C([O:8][C:9](=[O:21])[C:10]1[CH:15]=[CH:14][C:13]([C:16](=[NH:20])[N:17]([CH3:19])[CH3:18])=[CH:12][CH:11]=1)C.[OH-].[Li+]>O>[CH3:18][N:17]([CH3:19])[C:16]([C:13]1[CH:14]=[CH:15][C:10]([C:9]([OH:21])=[O:8])=[CH:11][CH:12]=1)=[NH:20]

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 22631319ethyl 4-(N,N-dimethylamidino)benzoate

生成物 1

HCID 4913141Prt-062802

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a THF solution of ethyl-4(N,N-dimethylcarbamimidoyl)benzoate (G) was added an aqueous solution of lithium hydroxide (2 eq.) and the reaction mixture was stirred for 6 hr. The completion of the reaction was confirmed by HPLC. To the reaction mixture was added water, followed by extraction with ethyl acetate. The aqueous layer was acidified with 6N HCl to pH between 3-4 at which point the desired 4-(N,N-dimethylcarbamimidoyl)benzoic acid precipitated as the white solid. The white solid isolated was washed with hexane to afford 4-(N,N-dimethylcarbamimidoyl)benzoic acid as an hydrochloride salt (A).

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. customprecipitated as the white solid
  3. customThe white solid isolated
  4. washwas washed with hexane

出典と根拠

ORDレコード
ord-391797919f5942c086431d568ef8cc1c
出典データセット
uspto-grants-2013_03
特許番号
US08394964B2

反応ノート

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