Benzyl Alcohol → HCID 70127773, 화합물

HRID 651378노트

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HRID 651378 반응식
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:4]=1[NH2:5].Cl[C:14]([O:16][CH2:17][C:18](Cl)(Cl)Cl)=[O:15].C(O)[C:23]1[CH:28]=[CH:27]C=[CH:25][CH:24]=1>C1COCC1>[CH2:17]([O:16][C:14](=[O:15])[NH:5][C:4]1[C:6]([N+:10]([O-:12])=[O:11])=[CH:7][CH:8]=[CH:9][C:3]=1[O:2][CH3:1])[C:18]1[CH:27]=[CH:28][CH:23]=[CH:24][CH:25]=1

참가 물질

5

반응물 3

HCID 244Benzyl AlcoholHCID 854916-Nitro-o-anisidineHCID 870632,2,2-Trichloroethyl chloroformate

생성물 1

HCID 70127773HCID 70127773, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a solution of 2-methoxy-6-nitroaniline (2g; 0.0119 moles) in anhydrous THF (20 ml), trichloroethyl chloroformate (1.43 ml; 0.01189 moles) was added dropwise. The reaction was heated for 45 minutes at 60° C., the solvent was then removed under vacuum and the crude residue was dissolved in dioxane (20 ml). To this solution, benzyl alcohol (2.46 ml; 0.0237 mmoles) was added and the reaction mixture was refluxed for 8 hours. The solvent was then removed under vacuum and the crude residue was poured into diluted 10% HCl. The title compound was extracted into ethyl ether. The crude brown oil was crystallized with diisopropyl ether to give a light brown solid. 1.9 g; m.p. 78-80° C.

후처리

  1. customthe solvent was then removed under vacuum
  2. dissolutionthe crude residue was dissolved in dioxane (20 ml)
  3. temperaturethe reaction mixture was refluxed for 8 hours
  4. customThe solvent was then removed under vacuum
  5. additionthe crude residue was poured
  6. additioninto diluted 10% HCl
  7. extractionThe title compound was extracted into ethyl ether
  8. customThe crude brown oil was crystallized with diisopropyl ether
  9. customto give a light brown solid

출처 및 근거

ORD 기록
ord-31ca015542f54f66a76b7a6966c24db7
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06281218B1

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