2,4-Dibromo-6-chloroaniline → HCID 22482744、化合物

HRID 2182072ノート

反応式

HRID 2182072 の反応式
[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([Br:9])[CH:5]=[C:4]([Br:10])[CH:3]=1.Br[CH2:12][C:13](=[C:15]([C:18]#[N:19])[C:16]#[N:17])[CH3:14]>C(O)(C)C.O1CCCC1>[NH2:19][C:18]1[N:8]([C:7]2[C:2]([Cl:1])=[CH:3][C:4]([Br:10])=[CH:5][C:6]=2[Br:9])[CH:12]=[C:13]([CH3:14])[C:15]=1[C:16]#[N:17]

参加物

5

反応物 2

HCID 42959822,4-Dibromo-6-chloroanilineHCID 10921206HCID 10921206、化合物

生成物 1

HCID 22482744HCID 22482744、化合物収率 26.3%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 5.3 g of 6-chloro-2,4-dibromoaniline and 3.5 g of 2-(2-bromo-1-methylethylidene)malononitrile was dissolved in a mixed solution of 10 ml of isopropanol and 10 ml of tetrahydrofuran. The reaction mixture was heated for 2 hours while being concentrated at 120° C. Water was poured into the reaction mixture. The reaction mixture was extracted with chloroform. The organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate and was dried over anhydrous sodium sulfate. After the desiccant was filtered off, the filtrate was concentrated under reduced pressure and was allowed to stand for crystallization to yield 1.9 g of 2-amino-4-methyl-1-(2,4-dibromo-6-chlorophenyl)pyrrole-3-carbonitrile.

後処理

  1. temperatureThe reaction mixture was heated for 2 hours
  2. concentrationwhile being concentrated at 120° C
  3. additionWater was poured into the reaction mixture
  4. extractionThe reaction mixture was extracted with chloroform
  5. washThe organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate
  6. dry with materialwas dried over anhydrous sodium sulfate
  7. filtrationAfter the desiccant was filtered off
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customto stand for crystallization

出典と根拠

ORDレコード
ord-3178361a09df47868d2776c702c15811
出典データセット
uspto-grants-2005_05
特許番号
US06894168B2

反応ノート

読み込み中…