Sodium Iodide → N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide

HRID 1958882ノート

反応式

HRID 1958882 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:10]=[CH:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[N:7]=1)=[O:4].[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O>[Cl:18][C:13]1[CH:12]=[C:11]([N:8]2[CH:9]=[CH:10][C:6]([NH:5][C:3](=[O:4])[CH2:2][N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[N:7]2)[CH:16]=[CH:15][C:14]=1[Cl:17]

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 8083MorpholineHCID 11430Potassium CarbonateHCID 577054132-chloro-N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)acetamide

生成物 1

HCID 24743570N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide収率 87.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-chloro-N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)acetamide (0.22 g, 0.74 mmol), morpholine (71 mg, 0.81 mmol), potassium carbonate (0.22 g, 1.62 mmol) and sodium iodide (0.11 g, 0.74 mmol) in dry dimethylformamide (5 ml) was stirred and warmed at 100° C., overnight, in a dry nitrogen atmosphere. The solvent was evaporated in vacuo and water was added to the crude residue. The dark solid precipitated was filtered and dried yielding a crude product purified by crystallization in ethyl acetate, and 0.23 g of N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide was obtained as a beige colour solid with m.p.=125-127° C.

後処理

  1. customThe solvent was evaporated in vacuo and water
  2. additionwas added to the crude residue
  3. customThe dark solid precipitated
  4. filtrationwas filtered
  5. customdried
  6. customyielding a crude product
  7. custompurified by crystallization in ethyl acetate

出典と根拠

ORDレコード
ord-52f897bef7384d609ac7015eafa40d33
出典データセット
uspto-grants-2013_04
特許番号
US08410159B2

反応ノート

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