Nitrogen → HCID 19824189, 화합물

HRID 728346노트

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HRID 728346 반응식
[N:1]#N.[S:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[C:8](Cl)=[O:9].Cl.N[C:13]1[CH:18]=[C:17]([CH:19]([CH3:21])[CH3:20])[C:16]([OH:22])=[C:15]([CH:23]([CH3:25])[CH3:24])[CH:14]=1.C(=O)([O-])O.[Na+]>C(Cl)Cl.O.C(OCC)(=O)C>[S:3]1[CH:7]=[CH:6][CH:5]=[C:4]1[C:8]([C:13]1[CH:18]=[C:17]([CH:19]([CH3:21])[CH3:20])[C:16]([OH:22])=[C:15]([CH:23]([CH3:25])[CH3:24])[C:14]=1[NH2:1])=[O:9]

참가 물질

8

반응물 4

HCID 947NitrogenHCID 789282-Thiophenecarbonyl chlorideHCID 516892Sodium BicarbonateHCID 678336004-Amino-2,6-di(propan-2-yl)phenol--hydrogen chloride (1/1)

생성물 1

HCID 19824189HCID 19824189, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

Under ice-cooling and N2 atmosphere, a solution of 1.47 g of 2-thiophenecarbonyl chloride in 10 ml of methylene chloride is added to a mixture of 2.91 g of 4-amino-2,6-diisopropylphenol hydrochloride, 90 ml of ethyl acetate, 80 ml of water, and 8.0 g of sodium hydrogen carbonate during a period of 30 minutes. After stirring at room temperature for one hour, organic layer is separated, washed with water, 10 % HCl, water, dried, and concentrated. The obtained solid is recrystallized from chloroform-hexane to give 1.7 g of 4-(2-thienylcarbonyl)-amino-2,6-diisopropylphenol.

후처리

  1. temperatureUnder ice-cooling
  2. customorganic layer is separated
  3. washwashed with water, 10 % HCl, water
  4. customdried
  5. concentrationconcentrated
  6. customThe obtained solid is recrystallized from chloroform-hexane

출처 및 근거

ORD 기록
ord-4688d2b2495a47dc93bd0a8228707901
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05047555

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