Sodium Carbonate → HCID 178513361, 화합물

HRID 1784544

반응식

HRID 1784544 반응식
[S:1]([C:5]1[S:9][C:8]([C:10]#[N:11])=[CH:7][CH:6]=1)(=[O:4])(=[O:3])[NH2:2].Cl.[NH2:13][OH:14].C(=O)([O-])[O-].[Na+].[Na+]>O.C(O)C>[OH:14][NH:13][C:10]([C:8]1[S:9][C:5]([S:1](=[O:4])(=[O:3])[NH2:2])=[CH:6][CH:7]=1)=[NH:11]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 220195265-Cyanothiophene-2-sulfonamide

생성물 1

HCID 178513361HCID 178513361, 화합물수율 58%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A stirred mixture of 5-sulfamoyl-thiophene-2-carbonitrile [CAS-No. 519055-65-3] (0.31 g, 1.65 mmol), hydroxylamine hydrochloride (0.23 g, 3.31 mmol) and sodium carbonate (0.175 g, 1.65 mmol) in water (4.6 ml) and ethanol (1 ml) was heated under reflux conditions for 1.5 h. The reaction mixture was poured into water (50 ml) and extracted with ethyl acetate (3×100 ml). The combined organic layers were washed with brine (100 ml), dried (MgSO4) and evaporated. The crude product was purified by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (ethyl acetate/MeOH/hexane) to yield the title compound (0.21 g, 58%) as a white solid. MS (ISN) 220.1 [(M−H)−]; mp 189° C.

후처리

  1. temperaturewas heated under reflux conditions for 1.5 h
  2. extractionextracted with ethyl acetate (3×100 ml)
  3. washThe combined organic layers were washed with brine (100 ml)
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe crude product was purified by flash chromatography on silica gel (ethyl acetate/heptane) and crystallization (ethyl acetate/MeOH/hexane)

출처 및 근거

ORD 기록
ord-c541337de22b4c3ba4b3ff8e6787cae7
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504404B2

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