Ethylamine → N-(2-Chloro-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide

HRID 53520

反応式

HRID 53520 の反応式
[CH2:1]([NH2:3])[CH3:2].Cl[C:5]1[C:10]([C:11]([NH:13][C:14]2[C:15]([Cl:21])=[N:16][CH:17]=[CH:18][C:19]=2[CH3:20])=[O:12])=[CH:9][CH:8]=[CH:7][N:6]=1.CCCCCC>C1(C)C(C)=CC=CC=1.C(OCC)(=O)C>[Cl:21][C:15]1[C:14]([NH:13][C:11]([C:10]2[C:5]([NH:3][CH2:1][CH3:2])=[N:6][CH:7]=[CH:8][CH:9]=2)=[O:12])=[C:19]([CH3:20])[CH:18]=[CH:17][N:16]=1

参加物

6

反応物 3

HCID 6341EthylamineHCID 8058HexaneHCID 104238682-Chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide

生成物 1

HCID 11066217N-(2-Chloro-4-methyl-3-pyridinyl)-2-ethylamino-3-pyridinecarboxamide収率 76.2%

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
165 °C

実験手順

Ethylamine (12.7 g) was added to a suspension of 21.0 g of the 2-chloro-N-(2-chloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide in 150 ml of xylene in a steel bomb. The mixture was then heated in an oil bath to 165° C. for 6 hrs. and then stirred overnight at room temperature. The solvent was removed in vacuo and water added to the residue. The product was extracted with ether, dried (sodium sulfate) and concentrated to give an oil. This was dissolved in ethyl acetate followed by hexane at which time a precipitate formed. The solid was filtered and dried to give 16.5 g of the title compound, m.p. 122°-124° C.

後処理

  1. customThe solvent was removed in vacuo and water
  2. additionadded to the residue
  3. extractionThe product was extracted with ether
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated
  6. customto give an oil
  7. customformed
  8. filtrationThe solid was filtered
  9. customdried

出典と根拠

ORDレコード
ord-6931056261934f4b9e2954d3c9e52c11
出典データセット
uspto-grants-1997_04
特許番号
US05620974

関連ノート

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