Ethanol → HCID 57901805, 화합물

HRID 1851439노트

반응식

HRID 1851439 반응식
[C:1]([C:3]1[NH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][C:6]=2[NH:12][S:13]([C:16]1[S:17][CH:18]=[CH:19][CH:20]=1)(=[O:15])=[O:14])#[N:2].Cl.[CH2:22]([O:24][C:25](=[O:30])[C@H:26]([CH2:28][SH:29])N)[CH3:23].C(O)C>O>[S:17]1[CH:18]=[CH:19][CH:20]=[C:16]1[S:13]([NH:12][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[NH:4][C:3]([C:1]1[S:29][CH2:28][CH:26]([C:25]([O:24][CH2:22][CH3:23])=[O:30])[N:2]=1)=[CH:11]2)(=[O:14])=[O:15]

참가 물질

5

반응물 3

HCID 702EthanolHCID 2723617Ethyl cysteinate hydrochlorideHCID 57901755HCID 57901755, 화합물

생성물 1

HCID 57901805HCID 57901805, 화합물수율 25.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of N-(2-cyano-1H-indol-7-yl)thiophene-2-sulfonamide (0.30 g), cysteine ethyl ester hydrochloride (0.22 g) and ethanol (10 mL) was heated under reflux overnight. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography and the title compound (0.11 g, yield 25%) was obtained as pale-yellow crystals from a fraction eluted with ethyl acetate-hexane (1:1, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point 156-157° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-331e1ea1d3884bf58b687c0fae4c21c5
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957070B2

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