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

HRID 53520

반응식

HRID 53520 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 8857Ethyl Acetate용매

반응 조건

온도
165 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6931056261934f4b9e2954d3c9e52c11
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620974

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