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Pyridine → Methyl 3-[(6-chloro-3-methyl-pyridine-2-carbonyl)amino]-2,4-dimethyl-benzoate

HRID 1427122
ノート
印刷プレビュー

反応式

HRID 1427122 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[C:5]([CH3:11])=[CH:4][CH:3]=1.[C:12](Cl)(=O)[C:13](Cl)=O.NC1(C)C=C(C)C=C([C:22]([O:24][CH3:25])=[O:23])C1.[N:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[CH2:37]1COCC1>C(Cl)Cl.CN(C)C1C=CN=CC=1.CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:31][C:36]2[C:12]([CH3:13])=[C:32]([CH:33]=[CH:34][C:35]=2[CH3:37])[C:22]([O:24][CH3:25])=[O:23])=[O:10])[C:5]([CH3:11])=[CH:4][CH:3]=1
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 1049PyridineHCID 8028TetrahydrofuranHCID 65578Oxalyl chlorideHCID 469414706-Chloro-3-methylpyridine-2-carboxylic acidHCID 86707353Methyl 3-amino-3,5-dimethylbenzoate

生成物 1

HCID 86707343Methyl 3-[(6-chloro-3-methyl-pyridine-2-carbonyl)amino]-2,4-dimethyl-benzoate収率 73%

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide触媒HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 6-chloro-3-methyl-pyridine-2-carboxylic acid (465 mg, 2.71 mmol) in THF (5 ml), CH2Cl2 (5 ml) and DMF (0.01 ml, 129.33 μmoles) is added dropwise oxalyl chloride (0.3 ml, 3.46 mmoles) at 0° C. and the reaction mixture is slowly allowed to warm to ambient temperature. After 2 hours, the solvent is removed under reduced pressure. To the residue CH2Cl2 (20 ml) is added and reaction mixture is cooled to 0° C., then methyl 3-amino-3,5-dimethylbenzoate (490 mg, 2.73 mmol) is added followed by N,N-dimethylpyridin-4-amine (15 mg, 122.78 μmoles) and pyridine (0.66 ml, 8.16 mmoles). The cooling bath is removed and the clear solution is allowed to warm to ambient temperature. After 1.5 hours, the solvent is removed and the reaction mixture is diluted with ethyl acetate and washed with 0.5N HCl, saturated solution of sodium bicarbonate, and brine. The organic layers are combined and dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure to give the title compound as a light yellow solid (664 mg, 73%). Mass spectrum (m/z): 333.2 (M+1).

後処理

  1. customthe solvent is removed under reduced pressure
  2. additionTo the residue CH2Cl2 (20 ml) is added
  3. customreaction mixture
  4. temperatureis cooled to 0° C.
  5. customThe cooling bath is removed
  6. temperatureto warm to ambient temperature
  7. waitAfter 1.5 hours
  8. customthe solvent is removed
  9. additionthe reaction mixture is diluted with ethyl acetate
  10. washwashed with 0.5N HCl, saturated solution of sodium bicarbonate, and brine
  11. dry with materialdried over anhydrous Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b2c75b51a33f467aa7c941e8efe34de9
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08933098B2

反応ノート

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