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Azobisisobutyronitrile → HCID 54207325, 화합물

HRID 2413227
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HRID 2413227 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[C:12]([CH3:13])=[CH:11][S:10][C:9]=2[CH:14]=1)=[O:4].[Br:15]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[C:12]([CH2:13][Br:15])=[CH:11][S:10][C:9]=2[CH:14]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 54127717HCID 54127717, 화합물

생성물 1

HCID 54207325HCID 54207325, 화합물수율 56.2%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

A mixture of 3-methylbenzo[b]thiophene-6-carboxylic acid methyl ester (1.03 g), N-bromosuccinimide (0.89 g), azobisisobutyronitrile (0.2 g) and carbon tetrachloride (25 ml) was heated under reflux for 2 hours and then cooled. The mixture was diluted with a few ml. of chloroform, washed with water, dried (Na2SO4) and evaporated to give a solid which was crystallized from ethyl acetate/petrol (b.p. 60°-80° C. to give 3-bromomethylbenzo[b]thiophene-6-carboxylic acid methyl ester (0.80 g), m.p. 108°-110° C.

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후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. temperaturecooled
  4. additionThe mixture was diluted with a few ml
  5. washof chloroform, washed with water
  6. dry with materialdried (Na2SO4)
  7. customevaporated
  8. customto give a solid which
  9. customwas crystallized from ethyl acetate/petrol (b.p. 60°-80° C.

출처 및 근거

ORD 기록
ord-3fbfee62a15c4c5bb6dbc45e3997810c
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04496572

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