1,2-Dichloroethane → HCID 13980725、化合物

HRID 461309ノート

反応式

HRID 461309 の反応式
C([C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=O)=[CH:15][CH:14]=2)[N:8]=1)CCCCC.[CH2:22](Cl)[CH2:23]Cl.P(Cl)(Cl)(Cl)=O>CCOCC>[CH2:9]([C:12]1[CH:11]=[N:10][C:9]([C:13]2[CH:14]=[CH:15][C:16]([C:17]#[N:19])=[CH:20][CH:21]=2)=[N:8][CH:7]=1)[CH2:13][CH2:14][CH2:15][CH2:22][CH3:23]

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 24813Phosphorus oxychlorideHCID 541836714-(4-n-Hexylpyrimid-2-yl)benzoic acid amide

生成物 1

HCID 13980725HCID 13980725、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

15.58 g. of 4-(4-n-hexylpyrimid-2-yl)benzoic acid amide are left in a mixture of 350 ml. of ethylene chloride and 5.58 ml. of phosphorus oxychloride for 90 minutes under reflux, with stirring. The reaction mixture, diluted with ether, is washed with 2N sodium hydroxide solution and then with water until neutral. After evaporation of the organic phase, drying over sodium sulfate, 14.6 g. of 5-n-hexyl-2-(4-cyanophenyl)pyrimidine result, which are distilled in high vacuum, m.p. 53.5° - 54.5°; cl.p. 35.5° - 36.5°.

後処理

  1. washis washed with 2N sodium hydroxide solution
  2. customAfter evaporation of the organic phase
  3. dry with materialdrying over sodium sulfate, 14.6 g

出典と根拠

ORDレコード
ord-37d61fc84d3a426d9c6824b870649a10
出典データセット
uspto-grants-1977_12
特許番号
US04062798

反応ノート

読み込み中…