Lithium hydroxide, monohydrate → HCID 178524946, 화합물

HRID 2170582노트

반응식

HRID 2170582 반응식
C([O:3][C:4]([C:6]1[C:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:12]=2[Cl:18])=[CH:9][NH:8][N:7]=1)=[O:5])C.O.[OH-].[Li+]>C1COCC1.O>[Cl:18][C:12]1[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:11]=1[C:10]1[C:6]([C:4]([OH:5])=[O:3])=[N:7][NH:8][CH:9]=1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 178470487HCID 178470487, 화합물

생성물 1

HCID 178524946HCID 178524946, 화합물수율 108.1%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

A solution of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid ethyl ester (205 mg; 0.72 mmol) and lithium hydroxide monohydrate (125 mg; 2.9 mmol) in 1:1 THF/water (10 ml) was heated at 60° C. overnight. The THF was removed by evaporation, the aqueous phase acidified with 1M hydrochloric acid then extracted with ethyl acetate (20 ml). The ethyl acetate layer was dried (MgSO4), filtered and evaporated to give 200 mg of 4-(2,4-dichloro-phenyl)-1H-pyrazole-3-carboxylic acid. (LC/MS: [M+H]+ 256.85).

후처리

  1. customThe THF was removed by evaporation
  2. extractionthen extracted with ethyl acetate (20 ml)
  3. dry with materialThe ethyl acetate layer was dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-3829806477864c69af8b3bf7396a6898
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051278B2

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