Dichloromethane → HCID 13560178、化合物

HRID 637828ノート

反応式

HRID 637828 の反応式
N#N.CN(C)CCC[C:8]1[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]=1[NH2:21].[CH2:23]([N:25]([CH2:28][CH3:29])[CH2:26]C)C.[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33](Cl)=[O:34].[CH2:40](Cl)Cl>>[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33]([NH:21][C:9]1[C:10]([N:14]([CH2:40][CH2:29][CH2:28][N:25]([CH3:23])[CH3:26])[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[N:11][CH:12]=[CH:13][CH:8]=1)=[O:34]

参加物

5

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 691102-Chlorobenzoyl chlorideHCID 86740554HCID 86740554、化合物

生成物 1

HCID 13560178HCID 13560178、化合物収率 74%

実験手順

To a stirred solution of 9 g (0.033 mole) of N2 -[3-(dimethylamino)propyl]-N2 -phenyl-2,3-pyridinediamine and 3.9 g (0.038 mole) triethylamine in 75 ml of dry methylene chloride was added dropwise with stirring at 15°-20° C., 6.4 g (0.037 mole) of 2-chlorobenzoyl chloride. After stirring overnight, the reaction mixture was washed with water. The methylene chloride layer was extracted twice with dilute sodium hydroxide solution, washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was triturated in isopropyl ether to give 10 g (74%) of solid. A portion of this solid was recrystallized from isopropyl alcohol-isopropyl ether to give a cream colored solid, m.p. 90°-92° C.

後処理

  1. stirringAfter stirring overnight
  2. washthe reaction mixture was washed with water
  3. extractionThe methylene chloride layer was extracted twice with dilute sodium hydroxide solution
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was triturated in isopropyl ether

出典と根拠

ORDレコード
ord-d74acf394c104f1fb3e08e99e7171ced
出典データセット
uspto-grants-1985_12
特許番号
US04558132

反応ノート

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