Diisopropylethylamine → N-(2-(4-(hydroxymethyl)piperidin-1-yl)ethyl)methanesulfonamide

HRID 53242

反応式

HRID 53242 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][OH:8])[CH2:3][CH2:2]1.C(N(CC)C(C)C)(C)C.Br[CH2:19][CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23]>C(#N)C>[OH:8][CH2:7][CH:4]1[CH2:5][CH2:6][N:1]([CH2:19][CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23])[CH2:2][CH2:3]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 285330N-(2-bromoethyl)methanesulfonamideHCID 4207714-Piperidinemethanol

生成物 1

HCID 19962114N-(2-(4-(hydroxymethyl)piperidin-1-yl)ethyl)methanesulfonamide収率 54.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

4-Piperidine methanol (1.60 g) was dissolved in dry acetonitrile (40 ml), N,N-diisopropylethylamine (5 ml) was added, followed by N-(2-bromoethyl)methanesulphonamide (2.95 g) in acetonitrile (10 ml), and the resulting mixture heated at reflux for 2 h. The solvent was removed in vacuo to leave a gum. This was purified by FCC eluting with System A (75:8:1) to give the title compound (1.80 g) as a solid, m.p. 81°-82°.

後処理

  1. temperaturethe resulting mixture heated
  2. temperatureat reflux for 2 h
  3. customThe solvent was removed in vacuo
  4. customto leave a gum
  5. customThis was purified by FCC
  6. washeluting with System A (75:8:1)

出典と根拠

ORDレコード
ord-b799967ecb2b40aeb1be5ec9736eebe1
出典データセット
uspto-grants-1997_04
特許番号
US05618827

関連ノート

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