Hydrochloric Acid → 2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid

HRID 604408노트

반응식

HRID 604408 반응식
C([O:3][C:4]([C:6]1[N:7]([CH2:16][C:17]2[CH:21]=[C:20]([C:22]3[S:23][C:24]([Cl:27])=[CH:25][CH:26]=3)[O:19][N:18]=2)[N:8]=[C:9]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=1)=[O:5])C.O.[OH-].[Li+].Cl>C1COCC1.O>[Cl:27][C:24]1[S:23][C:22]([C:20]2[O:19][N:18]=[C:17]([CH2:16][N:7]3[C:6]([C:4]([OH:5])=[O:3])=[CH:10][C:9]([C:11]4[S:12][CH:13]=[CH:14][CH:15]=4)=[N:8]3)[CH:21]=2)=[CH:26][CH:25]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 121509052-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid ethyl ester

생성물 1

HCID 121509062-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

To a solution of 4 g 2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid ethyl ester in 20 ml THF, 10 ml water and 500 mg lithium hydroxide monohydrate were added. After stirring for 2 h at 60° C. the reaction was cooled to RT. The mixture was acidified with half concentrated hydrochloric acid to pH 3 and the precipitate collected by filtration and washed with 10 ml water. The product was obtained as a white solid which was dried under reduced pressure. Yield: 3.8 g.

후처리

  1. temperaturewas cooled to RT
  2. filtrationthe precipitate collected by filtration
  3. washwashed with 10 ml water
  4. customThe product was obtained as a white solid which
  5. customwas dried under reduced pressure

출처 및 근거

ORD 기록
ord-6ac52f9602454f2aa88450406f7042c4
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07910606B2

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