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2-Aminophenol → 2H-1,4-benzoxazin-3(4H)-one

HRID 1587353
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HRID 1587353 반응식
Cl[CH2:2][C:3](Cl)=[O:4].[NH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13].[Cl-].C(C[NH3+])C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[O:4]=[C:3]1[NH:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[O:13][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 58012-AminophenolHCID 6577Chloroacetyl chlorideHCID 516892Sodium BicarbonateHCID 27505172-Phenylethylazanium;chloride

생성물 1

HCID 727572H-1,4-benzoxazin-3(4H)-one수율 32.2%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A solution of chloroacetyl chloride (31.2 g) in chloroform (100 ml) was added dropwise to a mixture of 2-aminophenol (25 g), benzylmethylammonium chloride (52.4 g), sodium bicarbonate (77 g) and chloroform (500 ml) which was cooled in an ice-bath. The mixture was stirred for 1 hour and allowed to warm to ambient temperature. The mixture was heated to 55° C. for 5 hours and then stirred at ambient temperature for 16 hours. The mixture was evaporated and the residue was partitioned between ethyl acetate and an aqueous solution of potassium carbonate. The organic phase was washed with dilute aqueous hydrochloric acid and with water, dried (MgSO4) and evaporated. The residue was washed with a mixture of hexane and diethyl ether to leave 3-oxo-2,3-dihydro-4H-1,4-benzoxazine (11 g, 32%) m.p. 172°-173° C.

후처리

  1. temperaturewas cooled in an ice-bath
  2. temperatureThe mixture was heated to 55° C. for 5 hours
  3. stirringstirred at ambient temperature for 16 hours
  4. customThe mixture was evaporated
  5. customthe residue was partitioned between ethyl acetate
  6. washThe organic phase was washed with dilute aqueous hydrochloric acid and with water
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. washThe residue was washed with a mixture of hexane and diethyl ether

출처 및 근거

ORD 기록
ord-1657c5a9001f4a409b12d7048f1d9f2c
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05217969

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