Hydrochloric Acid → ethyl 7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate

HRID 1851498노트

반응식

HRID 1851498 반응식
COC[N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[N:13]([CH3:22])[S:14]([C:17]2[S:18][CH:19]=[CH:20][CH:21]=2)(=[O:16])=[O:15])[CH:6]=[C:5]1[C:23]([O:25][CH2:26][CH3:27])=[O:24].Cl.C(O)C>O>[CH3:22][N:13]([S:14]([C:17]1[S:18][CH:19]=[CH:20][CH:21]=1)(=[O:15])=[O:16])[C:11]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:12]=1[NH:4][C:5]([C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:6]2

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 57475950ethyl 1-(methoxymethyl)-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate

생성물 1

HCID 57475952ethyl 7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate수율 46%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of ethyl 1-(methoxymethyl)-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxylate (1.06 g), concentrated hydrochloride (1 mL) and ethanol (5 mL) was heated under reflux overnight. Water was added to the reaction mixture, and the obtained crystals were filtrated, washed with water and dried. The obtained crystals were subjected to silica gel column chromatography and the title compound (0.43 g, yield 46%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (2:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 164-165° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. filtrationthe obtained crystals were filtrated
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-d0a8669319174e4c860d6b93075ec478
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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