Dichloromethane → 3-Aminopyrazine-2-carboxylic acid 2-chlorophenylamide

HRID 430516

反応式

HRID 430516 の反応式
[NH2:1][C:2]1[C:3]([C:8]([OH:10])=O)=[N:4][CH:5]=[CH:6][N:7]=1.C(Cl)Cl.[Cl:14][C:15]1[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=1[NH2:17].Cl.CN(C)CCCN=C=NCC>CN(C)C1C=CN=CC=1.CN(C)C=O>[Cl:14][C:15]1[CH:21]=[CH:20][CH:19]=[CH:18][C:16]=1[NH:17][C:8]([C:3]1[C:2]([NH2:1])=[N:7][CH:6]=[CH:5][N:4]=1)=[O:10]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 72402-ChloroanilineHCID 726563-Amino-2-pyrazinecarboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 540969723-Aminopyrazine-2-carboxylic acid 2-chlorophenylamide収率 50%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 3-aminopyrazine carboxylic acid (7.0 g, 50.32 mmol), methylene chloride (60 mL), dimethylformamide (40 mL), 4-dimethylaminopyridine (15.37 g, 126 mmol), 2-chloroaniline (5.82 mL, 55.35 mmol), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (11.58 g, 60.38 mmol) was stirred overnight at ambient temperature. The solvent was removed and the residue was mixed with ethyl acetate and 1 N lithium chloride. The precipitate which formed was filtered and rinsed with 1 N lithium chloride, ethyl acetate, and ether and then air dried to afford 6.22 g (50%) of 3-aminopyrazine-2-carboxylic acid 2-chlorophenylamide as fluffy yellow crystals.

後処理

  1. customThe solvent was removed
  2. additionthe residue was mixed with ethyl acetate and 1 N lithium chloride
  3. customThe precipitate which formed
  4. filtrationwas filtered
  5. washrinsed with 1 N lithium chloride, ethyl acetate, and ether
  6. customair dried

出典と根拠

ORDレコード
ord-6896b7fd7f444ab7bda70b4c478c1ee7
出典データセット
uspto-grants-2001_11
特許番号
US06323208B1

関連ノート

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