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Water → 7-Aminocarbonyl-6-chloro-2,3-dihydro-2,2-dimethylbenzofuran

HRID 52648
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HRID 52648 반응식
[Cl:1][C:2]1[CH:12]=[CH:11][C:5]2[CH2:6][C:7]([CH3:10])([CH3:9])[O:8][C:4]=2[C:3]=1[C:13]#[N:14].[OH-:15].[K+].O>CC(O)(C)C>[NH2:14][C:13]([C:3]1[C:4]2[O:8][C:7]([CH3:10])([CH3:9])[CH2:6][C:5]=2[CH:11]=[CH:12][C:2]=1[Cl:1])=[O:15]
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참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 538583176-Chloro-7-cyano-2,3-dihydro-2,2-dimethylbenzofuran

생성물 1

HCID 539852047-Aminocarbonyl-6-chloro-2,3-dihydro-2,2-dimethylbenzofuran수율 75.7%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A stirred solution of 10.0 grams (0.048 mole) of 6-chloro-7-cyano-2,3-dihydro-2,2-dimethylbenzofuran in 200 mL of 2-methyl-2-propanol was warmed to reflux, and 9.5 grams (0.17 mole) of 85% potassium hydroxide was added in one portion. Upon completion of addition, the reaction mixture was heated at reflux for about 75 minutes. The reaction mixture was then cooled and poured into 400 mL of water that was cooled in an ice bath. The resultant solid was collected by filtration and dried under vacuum, yielding 8.2 grams of 7-aminocarbonyl-6-chloro-2,3-dihydro-2,2-dimethylbenzofuran. The NMR spectrum was consistent with the proposed structure.

후처리

  1. temperatureto reflux
  2. additionUpon completion of addition
  3. temperaturethe reaction mixture was heated
  4. temperatureat reflux for about 75 minutes
  5. temperatureThe reaction mixture was then cooled
  6. temperaturewas cooled in an ice bath
  7. filtrationThe resultant solid was collected by filtration
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-5848710eda984d9493a565b51dc463b4
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05616718

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