Triethylamine → 1-(Methanesulfonyl)-4-methylpiperazine

HRID 1090351ノート

反応式

HRID 1090351 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:15][S:16](Cl)(=[O:18])=[O:17]>O1CCCC1.C(OCC)(=O)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:16]([CH3:15])(=[O:18])=[O:17])[CH2:4][CH2:3]1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2 回HCID 531671-Methylpiperazine

生成物 1

HCID 8177701-(Methanesulfonyl)-4-methylpiperazine

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

A mixture of N-methylpiperazine (3.0 g, 29.9 mmol), triethylamine (3.6 g, 35.9 mmol) and methanesulfonyl chloride (Compound 19, 4.11 g, 35.9 mmol) in tetrahydrofuran (20 ml) was stirred at 0° C. for 2 hours. The mixture was filtered and the filtrate was evaporated to dryness to give a solid. The solid was redissolved in ethyl acetate and washed with water. Evaporation of the dried (magnesium sulfate) organic phase gave the title sulfonamide. 1HNMR(CDCl3): 2.35 (s, 3H), 2.53 (t, 4H, J=5.0 Hz), 2.79 (s, 3H) and 3.27 (t, 4H, J=5.0 Hz).

後処理

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated to dryness
  3. customto give a solid
  4. washwashed with water
  5. customEvaporation of the
  6. dry with materialdried (magnesium sulfate) organic phase

出典と根拠

ORDレコード
ord-64a6c1fc458b4e65b8b1b9e06ea89865
出典データセット
uspto-grants-1992_01
特許番号
US05081261

反応ノート

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