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Hydrochloric Acid → HCID 11610770, 화합물

HRID 1883472
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HRID 1883472 반응식
[CH3:1][N:2]1[CH:6]=[C:5]([NH:7][C:8]([O:10][CH2:11][CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)=[O:9])[CH:4]=[C:3]1[C:24]([O:26]C)=[O:25].[Li+].[OH-].Cl>C1COCC1.O>[CH3:1][N:2]1[CH:6]=[C:5]([NH:7][C:8]([O:10][CH2:11][CH2:12][S:13][C:14]2[CH:15]=[CH:16][C:17]([C:20]([F:23])([F:21])[F:22])=[CH:18][CH:19]=2)=[O:9])[CH:4]=[C:3]1[C:24]([OH:26])=[O:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 11188835HCID 11188835, 화합물

생성물 1

HCID 11610770HCID 11610770, 화합물수율 66.3%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

Methyl 1-methyl-4-[2-(4-trifluoromethyl-phenylsulfanyl)-ethoxycarbonylamino]-1H-pyrrole-2-carboxylate (5.0 g, 12.43 mmol) prepared in the capping step was dissolved in THF/H2O (200 ml/100 ml), 1N LiOH (30 ml) was added thereto, and the mixture was stirred for 4 days at room temperature. The reaction solution was acidified to pH 2.0 by 1N HCl and then extracted with EA and water. The organic layer was washed with aqueous NaCl solution and dried over anhydrous MgSO4. The solvent contained therein was removed to give a white solid, which was then recrystallized from EA and n-hexane to give 1-methyl-4-[2-(4-trifluoromethyl-phenylsulfanyl)-ethoxy carbonylamino]-1H-pyrrole-2-carboxylic acid (3.20 g, 66.29%) of a pale yellow solid.

후처리

  1. extractionextracted with EA and water
  2. washThe organic layer was washed with aqueous NaCl solution
  3. dry with materialdried over anhydrous MgSO4
  4. customThe solvent contained therein was removed
  5. customto give a white solid, which
  6. customwas then recrystallized from EA and n-hexane

출처 및 근거

ORD 기록
ord-de65d8c947f24d2e88031a2a0b78f336
출처 데이터셋
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06759511B2

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