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

HRID 2096712
ノート
印刷プレビュー

反応式

HRID 2096712 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide触媒HCID 111,2-Dichloroethane溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

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+].

後処理

  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)

出典と根拠

ORDレコード
ord-bc28f390f0f54ba4ab1c9396df5437fd
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08450313B2

反応ノート

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