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Water → 2-Bromo-5-isocyanato-1,3-dimethylbenzene

HRID 1754970
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HRID 1754970 반응식
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[Br:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([NH2:21])=[CH:16][C:15]=1[CH3:22].O>O1CCOCC1>[Br:13][C:14]1[C:19]([CH3:20])=[CH:18][C:17]([N:21]=[C:5]=[O:11])=[CH:16][C:15]=1[CH3:22]
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참가 물질

5

반응물 3

HCID 962WaterHCID 94429TriphosgeneHCID 123831174-Bromo-3,5-dimethylaniline

생성물 1

HCID 866727652-Bromo-5-isocyanato-1,3-dimethylbenzene수율 117.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

Triphosgene (2.23 g, 7.52 mmol) was added to a solution of 4-bromo-3,5-dimethyl-phenylamine (4.3 g, 21.49 mmol) in dioxane (71 ml). After stirring at 100° C. for 15 hours, water was added to the reaction solution. After extraction with ethyl acetate, the organic phase was sequentially washed with water and saturated brine and concentrated under reduced pressure to give 2-bromo-5-isocyanato-1,3-dimethylbenzene (2.0 g, 41%).

후처리

  1. extractionAfter extraction with ethyl acetate
  2. washthe organic phase was sequentially washed with water and saturated brine
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-fb602089dde1444fa16869f3eea4d148
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169254B2

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