Potassium Carbonate → 9H-Thioxanthen-9-one, 1-[[2-(dimethylamino)ethyl]amino]-4-nitro-

HRID 1380614ノート

反応式

HRID 1380614 の反応式
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH2:5].Cl[C:8]1[C:21]2[C:20](=[O:22])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[S:13][C:12]=2[C:11]([N+:23]([O-:25])=[O:24])=[CH:10][CH:9]=1.C([O-])([O-])=O.[K+].[K+]>C1(C)C(C)=CC=CC=1>[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][NH:5][C:8]1[C:21]2[C:20](=[O:22])[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[S:13][C:12]=2[C:11]([N+:23]([O-:25])=[O:24])=[CH:10][CH:9]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 66053N,N-Dimethylethylenediamine2 回HCID 12909396HCID 12909396、化合物

生成物 1

HCID 3296019H-Thioxanthen-9-one, 1-[[2-(dimethylamino)ethyl]amino]-4-nitro-収率 85.6%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

A solution of 9.3 g (0.105 mole) of N,N-dimethylethylenediamine in 35 ml of xylene was added dropwise over ten minutes to a stirred mixture of 1-chloro-4-nitrothioxanthone (24.5 g, 0.084 mole) and K2CO3 (12.2 g, 0.088 mole) in 350 ml of xylene. The mixture was heated for one hour at 70°, an additional 1.8 g (0.088 mole) of N,N-dimethylethylendiamine was added, and heating was continued for an additional hour. The mixture was cooled and the solid was collected, washed with cold xylene, petroleum ether, dried, triturated with water, and dried in vacuo at 70° to give the product (24.7 g) as a yellow solid, mp 177°-179°.

後処理

  1. temperatureThe mixture was heated for one hour at 70°
  2. temperatureheating
  3. waitwas continued for an additional hour
  4. temperatureThe mixture was cooled
  5. customthe solid was collected
  6. washwashed with cold xylene, petroleum ether
  7. customdried
  8. customtriturated with water
  9. customdried in vacuo at 70°

出典と根拠

ORDレコード
ord-5da7bd0770b34a0f955ea7401c71917a
出典データセット
uspto-grants-1986_04
特許番号
US04582851

反応ノート

読み込み中…