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Hydrochloric Acid → 6-[2-(2-chloro-5-methoxy-phenyl)-acetyl]-4-methyl-4H-benzo[1,4]oxazin-3-one

HRID 2386693
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HRID 2386693 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][C:11]([OH:13])=O.C(Cl)(=O)C(Cl)=O.[CH3:20][N:21]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[O:24][CH2:23][C:22]1=[O:31].[Al+3].[Cl-].[Cl-].[Cl-].Cl>O1CCCC1.CN(C)C=O.ClCCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][C:11]([C:28]1[CH:29]=[CH:30][C:25]2[O:24][CH2:23][C:22](=[O:31])[N:21]([CH3:20])[C:26]=2[CH:27]=1)=[O:13]
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참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 65578Oxalyl chlorideHCID 890322H-1,4-Benzoxazin-3(4H)-one,4-methyl-HCID 6451240Aluminum(III) ChlorideHCID 153659582-(2-Chloro-5-methoxyphenyl)acetic acid

생성물 1

HCID 666972226-[2-(2-chloro-5-methoxy-phenyl)-acetyl]-4-methyl-4H-benzo[1,4]oxazin-3-one
수율 92.8%

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매HCID 111,2-Dichloroethane용매2회HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (2-chloro-5-methoxy-phenyl)-acetic acid (1 g) in tetrahydrofuran (20 ml) were added N,N-dimethylformamide (2 drops) and oxalylchloride (1.03 g). The mixture was stirred overnight at room temperature. The solvent was evaporated; toluene was added and again evaporated. The residue was dried under high vacuum to give the crude acid chloride. To a cooled solution (ice bath) of 4-methyl-2H-1,4-benzoxazin-3(4H)-one (830 mg) in 1,2-dichloroethane (5 ml) was added AlCl3 (1.99 g). The mixture was stirred for 10 min and a solution of the acid chloride in 1,2-dichloroethane (5 ml) was added dropwise. The mixture was stirred at 0° C. for 4.5 h. The mixture was poured into ice water and hydrochloric acid and extracted with dichloromethane. The organic phase was dried (MgSO4), filtered and concentrated. The product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>0:1) to give the title compound (1.6 g) as an off-white solid. MS (m/e)=346.1 [M+H+].

후처리

  1. customThe solvent was evaporated
  2. additiontoluene was added
  3. customagain evaporated
  4. customThe residue was dried under high vacuum
  5. customto give the crude acid chloride
  6. stirringThe mixture was stirred for 10 min
  7. stirringThe mixture was stirred at 0° C. for 4.5 h
  8. extractionextracted with dichloromethane
  9. dry with materialThe organic phase was dried (MgSO4)
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customThe product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>0:1)

출처 및 근거

ORD 기록
ord-8342743b08eb44c9a68b0c0564aadc66
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268820B2

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