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Hydrochloric Acid → HCID 18543276, 화합물

HRID 990871
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HRID 990871 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][CH2:10][C:11]#[N:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.O.Cl.[OH-].[Na+]>COCCOC>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][CH2:10][CH2:11][NH2:12])[CH:3]=[C:2]([Cl:1])[CH:7]=1
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 18543019(3,5-Dichlorophenylthio)acetonitrile

생성물 1

HCID 18543276HCID 18543276, 화합물수율 81.8%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of (3,5-dichlorophenylthio)acetonitrile (1.2 g) in 3.0 mL of ethylene glycol dimethyl ether is added 0.61 mL of 10M borne dimethyl sulfide complex and the mixture heated at reflux for 0.5 hours. The reaction is cooled in an ice bath and 2.0 mL of water and 2.0 mL of concentrated hydrochloric acid is added. This mixture is heated at reflux for 0.5 hr. The clear solution is then cooled and basified with 5N sodium hydroxide and extracted with ether. The ether extract is dried over potassium carbonate, filtered and concentrated to give 1.0 g of a colorless oil.

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 0.5 hours
  3. temperatureThe reaction is cooled in an ice bath
  4. temperatureThis mixture is heated
  5. temperatureat reflux for 0.5 hr
  6. temperatureThe clear solution is then cooled
  7. extractionextracted with ether
  8. extractionThe ether extract
  9. dry with materialis dried over potassium carbonate
  10. filtrationfiltered
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d4ac9e3d476b4c87ac2e3f5770222e32
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06462055B2

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