2-Chloro-4-nitroaniline → HCID 4715112, 화합물

HRID 2290545노트

반응식

HRID 2290545 반응식
[Cl:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[NH2:4].CO[CH:14]1[CH2:18][CH2:17][CH:16](OC)O1>C(O)(=O)C.O>[Cl:1][C:2]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:3]=1[N:4]1[CH:14]=[CH:18][CH:17]=[CH:16]1

참가 물질

5

반응물 2

HCID 84922-Chloro-4-nitroanilineHCID 790982,5-Dimethoxytetrahydrofuran

생성물 1

HCID 4715112HCID 4715112, 화합물수율 84.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A stirred mixture of 20.0 g (0.12 mole) of 2-chloro-4-nitroaniline and 17.9 g (0.14 mole) of 2,5-dimethoxytetrahydrofuran in 30 ml of glacial acetic acid was heated at reflux for three hours. The mixture was cooled to room temperature, diluted with water, and extracted with diethyl ether. The extract was washed with a saturated aqueous potassium carbonate solution then dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated from the filtrate under reduced pressure to leave a solid. The solid was purified by recrystallization from methylcyclohexane to yield 22.5 g of 1-(2-chloro-4-nitrophenyl)pyrrole (mp 54°-55° C.).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for three hours
  3. extractionextracted with diethyl ether
  4. washThe extract was washed with a saturated aqueous potassium carbonate solution
  5. dry with materialthen dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customThe solvent was evaporated from the filtrate under reduced pressure
  8. customto leave a solid
  9. customThe solid was purified by recrystallization from methylcyclohexane

출처 및 근거

ORD 기록
ord-2e475199f5ac44afba814ec57ad23690
출처 데이터셋
uspto-grants-1986_10
특허 번호
US04617316

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