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Ethyl 4,4-difluoroacetoacetate (30.12 g, 0.172 mol) was stirred in toluene (600 mL) over ice water. Solution of N-methylhydrazine (7.6 mL, 0.14 mol) in toluene (200 mL) was added slowly, dropwise over 20 min. The reaction mixture was heated at 100° C. for 2 hours. The reaction mixture evaporated to dryness. The resulting material was triturated with methyl t-butylether/heptane to give 3-(difluoromethyl)-1-methyl-1H-pyrazol-5(4H)-one in three batches (total 10.7 g, 51%) as orange powder. This mat
| 产品 | |
| 反应物 |
ethyl difluoroacetoacetate ice methylhydrazine |
| 试剂 |
toluene toluene |
| 程序 |
1、Stir Ethyl 4,4-difluoroacetoacetate (30.12 g, 0.172 mol) was stirred in toluene (600 mL) over ice water 2、Add Solution of N-methylhydrazine (7.6 mL, 0.14 mol) in toluene (200 mL) was added slowly, dropwise over 20 min 3、Heat The reaction mixture was heated at 100° C. for 2 hours 4、Remove The reaction mixture evaporated to dryness 5、Purify The resulting material was triturated with methyl t-butylether/heptane 6、Yield to give 3-(difluoromethyl)-1-methyl-1H-pyrazol-5(4H)-one in three batches (total 10.7 g, 51%) as orange powder |
角色：product
分类：产品
实体类型：exact
角色：reactant
分类：原料
实体类型：exact
角色：reactant
分类：原料
实体类型：exact
角色：reactant
分类：原料
实体类型：exact
角色：solvent
分类：催化剂
实体类型：exact
角色：solvent
分类：催化剂
实体类型：exact