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Triethylamine → N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-chloro-benzenesulfonamide

HRID 378287
ノート
印刷プレビュー

反応式

HRID 378287 の反応式
[Cl: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][CH3:20])[N:13]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.CN.[CH2:24]([N:26](CC)CC)C>C(O)C>[CH3:20][NH:19][C:14]1[N:13]=[C:12]([NH:11][S:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)(=[O:10])=[O:9])[CH:17]=[C:16]([NH:26][CH3:24])[N:15]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6364545Methylamine hydrochlorideHCID 193535554-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide

生成物 1

HCID 17774528N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-chloro-benzenesulfonamide収率 45%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
140 °C

実験手順

0.62 g (0.0019 mol) of 4-chloro-N-(6-chloro-2-methylamino-pyrimidin-4-yl)-benzenesulfonamide was dissolved in 10 ml of ethanol, treated with 1.67 g (0.025 mol) of methylamine hydrochloride and 6.2 ml (0.044 mol) of triethylamine and stirred in an autoclave at 140° C. for 18 hours. The mixture was freed completely from solvent, the residue was partitioned in ethyl acetate/water and the insoluble constituents were filtered off under suction. The filter cake was recrystallized in methanol/diethyl ether. There was obtained 0.28 g (45%) of N-(2,6-bis-methylamino-pyrimidin-4-yl)-4-chloro-benzenesulfonamide as white crystals; m.p. 272-273° C.

後処理

  1. customthe residue was partitioned in ethyl acetate/water
  2. filtrationthe insoluble constituents were filtered off under suction
  3. customThe filter cake was recrystallized in methanol/diethyl ether

出典と根拠

ORDレコード
ord-b19d8bc201604946b3d9f6e15227402e
出典データセット
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06030976

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート