Methanesulfonyl chloride → N-{4-[4-(Pyridin-4-yl)piperazin-1-yl]phenyl}methanesulfonamide

HRID 2232396

反応式

HRID 2232396 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:18][CH2:17][N:16]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=3)[CH2:15][CH2:14]2)=[CH:9][CH:8]=1>N1C=CC=CC=1>[N:22]1[CH:23]=[CH:24][C:19]([N:16]2[CH2:15][CH2:14][N:13]([C:10]3[CH:11]=[CH:12][C:7]([NH:6][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:8][CH:9]=3)[CH2:18][CH2:17]2)=[CH:20][CH:21]=1

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 108904611-(4-Aminophenyl)-4-(4-pyridyl)piperazine

生成物 1

HCID 15735407N-{4-[4-(Pyridin-4-yl)piperazin-1-yl]phenyl}methanesulfonamide収率 42.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methanesulphonyl chloride (0.50 g) was added dropwise to a stirred solution of 1-(4-aminophenyl)-4-(4-pyridyl)piperazine (1.00 g) in dry pyridine (10 ml) at room temperature. The mixture was stirred at room temperature for 20 hours and then evaporated. The residue was dissolved in water and the solution was basified with sodium bicarbonate solution and allowed to stand for 2 hours. The solid was filtered off, washed with water, dried and crystallised from methanol/ethyl acetate to give the title compound (0.55 g), m.p. 230°-232° C. Found: C,57.80; H,6.07; N,16.89. C16H20N4O2S requires: C,57.81; H,6.06; N,16.85%.

後処理

  1. customevaporated
  2. dissolutionThe residue was dissolved in water
  3. waitto stand for 2 hours
  4. filtrationThe solid was filtered off
  5. washwashed with water
  6. customdried
  7. customcrystallised from methanol/ethyl acetate

出典と根拠

ORDレコード
ord-4c8f5d71fb2241cbb014594916a86f98
出典データセット
uspto-grants-1988_11
特許番号
US04788196

関連ノート

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