Trimethylamine → 4-amino-N-(2-ethylamino-6-methylamino-pyrimidin-4-yl)-benzenesulfonamide

HRID 378272ノート

反応式

HRID 378272 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16](Cl)[N:15]=[C:14]([NH:19][CH2:20][CH3:21])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:22][N:23](C)C.Cl.CN>C(O)C>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:17]=[C:16]([NH:23][CH3:22])[N:15]=[C:14]([NH:19][CH2:20][CH3:21])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 1146TrimethylamineHCID 6364545Methylamine hydrochlorideHCID 108300934-amino-N-(6-chloro-2-ethylamino-pyrimidin-4-yl)-benzenesulfonamide

生成物 1

HCID 107109724-amino-N-(2-ethylamino-6-methylamino-pyrimidin-4-yl)-benzenesulfonamide収率 54%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

0.1 g (0.00031 mol) of 4-amino-N-(6-chloro-2-ethylamino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in 20 ml of ethanol and stirred with 0.6 ml (0.0043 mol) of trimethylamine and 0.1 g (0.0015 mol) of methylamine hydrochloride in an autoclave at 130° C. for 4 hours. The reaction mixture was freed from solvent, the residue was suspended in 5 ml of ethanol and treated in an ultrasound bath for 15 minutes. The precipitate was filtered off, dissolved in 150 ml of 1N NaOH and filtered. The filtrate was adjusted to pH 6 with 0.1N HCl. The precipitate was filtered off under suction, washed with water and dried. There was obtained 0.053 g (54%) of 4-amino-N-(2-ethylamino-6-methylamino-pyrimidin-4-yl)-benzenesulfonamide as beige crystals; m.p.: 261-263° C.

後処理

  1. additiontreated in an ultrasound bath for 15 minutes
  2. filtrationThe precipitate was filtered off
  3. dissolutiondissolved in 150 ml of 1N NaOH
  4. filtrationfiltered
  5. filtrationThe precipitate was filtered off under suction
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-2e4f447117ae4b1f96b12df214385e9c
出典データセット
uspto-grants-2000_02
特許番号
US06030976

反応ノート

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