Lithium Hydroxide → Prt-062802

HRID 878418노트

반응식

HRID 878418 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 4913141Prt-062802

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-064179408f2c43e18029a0888d5a5823
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987463B2

반응 노트

불러오는 중…