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Hydrogen Bromide → HCID 59264693, 화합물

HRID 646406
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HRID 646406 반응식
[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[CH:9][C:8]([C:11](=[S:13])[NH2:12])=[CH:7][CH:6]=1)[CH3:2].Br[CH2:16][C:17]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)=O.Br>C(O)(C)C.C(OCC)C>[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[CH:9][C:8]([C:11]2[S:13][CH:16]=[C:17]([C:19]3[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=3)[N:12]=2)=[CH:7][CH:6]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 260Hydrogen BromideHCID 1514083-(2-Bromoacetyl)pyridineHCID 54189111Ethyl 4-(aminothioxomethyl)benzoate

생성물 1

HCID 59264693HCID 59264693, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 3776Isopropanol용매

실험 절차

4-Thiocarbamoyl-benzoic acid ethyl ester (CAS 78950-31-9) (0.4 g, 1.91 mmol), and 2-Bromo-1-pyridin-3-yl-ethanone; hydrobromide (CAS 17694-68-7) (0.537 g, 1.91 mmol) is placed in a 100 mL flask and dissolved in 20 mL of isopropyl alcohol. The mixture is heated to reflux for 1.5 hours and cooled and diluted with 40 mL of diethyl ether. The resulting solid is filtered and dissolved in a mixture of dichloromethane and saturated sodium bicarbonate solution. The organics are separated, dried over sodium sulfate, filtered and concentrated to provide 0.565 g of the titled compound. MS (m/e) 311.1 (M+1)

후처리

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 1.5 hours
  3. temperaturecooled
  4. filtrationThe resulting solid is filtered
  5. dissolutiondissolved in a mixture of dichloromethane and saturated sodium bicarbonate solution
  6. customThe organics are separated
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8b743cc858d344dfb2b1f7946183dce0
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07705025B2

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