Diisopropyl Ether → N-(1,5-dimethylpyrazol-3-yl)-2,6 dimethyl benzamide

HRID 128724

反応式

HRID 128724 の反応式
[NH2:1][C:2]1[CH:6]=[C:5]([CH3:7])[N:4]([CH3:8])[N:3]=1.[CH3:9][C:10]1[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[C:11]=1[C:12](Cl)=[O:13].C([O-])(O)=O.[Na+].C(OC(C)C)(C)C>C(Cl)Cl.CCOC(C)=O>[CH3:8][N:4]1[C:5]([CH3:7])=[CH:6][C:2]([NH:1][C:12](=[O:13])[C:11]2[C:15]([CH3:19])=[CH:16][CH:17]=[CH:18][C:10]=2[CH3:9])=[N:3]1

参加物

7

反応物 4

HCID 7914Diisopropyl EtherHCID 890962,6-Dimethylbenzoyl chlorideHCID 516892Sodium BicarbonateHCID 70177471,5-dimethyl-1H-pyrazol-3-amine

生成物 1

HCID 11776550N-(1,5-dimethylpyrazol-3-yl)-2,6 dimethyl benzamide収率 38.2%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a cooled (0°-5° C.) solution of 3-amino-1,5-dimethyl pyrazole (95%, 32.7 g, 0.28M) in anhydrous CH2Cl2 (200 ml) was added a CH2Cl2 (100 ml) solution of the 2,6 dimethyl benzoyl chloride (23.6 g, 0.14M). The reaction mixture was allowed to room temperature for 18 hours and then CH2Cl2 was concentrated to give an oily mixture which was diluted in AcOEt. This suspension was then treated with saturated NaHCO3. After usual work-up, the crude material was cristallized with diisopropyloxide to give 13 g of the desired amide (38% : yield based on the 2,6-dimethyl benzoyl chloride).

後処理

  1. concentrationCH2Cl2 was concentrated
  2. customto give an oily mixture which

出典と根拠

ORDレコード
ord-f98ffc91eb5e435fac5c17e51ecfdfc5
出典データセット
uspto-grants-1995_11
特許番号
US05464860

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