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Iodoethane → N-[4-(cyclopropylmethoxy)phenylmethyl]-N-ethoxy-4-[bis(4-trifluoromethylphenyl)hydroxymethyl]-piperidinium iodide

HRID 482281
ノート
印刷プレビュー

反応式

HRID 482281 の反応式
[CH:1]1([CH2:4][O:5][C:6]2[CH:11]=[CH:10][C:9]([CH2:12][N+:13]3([O-:41])[CH2:18][CH2:17][CH:16]([C:19]([C:31]4[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:39])[F:38])=[CH:33][CH:32]=4)([C:21]4[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=4)[OH:20])[CH2:15][CH2:14]3)=[CH:8][CH:7]=2)[CH2:3][CH2:2]1.[CH2:42]([I:44])[CH3:43]>C(#N)C>[I-:44].[CH:1]1([CH2:4][O:5][C:6]2[CH:11]=[CH:10][C:9]([CH2:12][N+:13]3([O:41][CH2:42][CH3:43])[CH2:14][CH2:15][CH:16]([C:19]([C:31]4[CH:36]=[CH:35][C:34]([C:37]([F:38])([F:39])[F:40])=[CH:33][CH:32]=4)([C:21]4[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:28])[F:29])=[CH:23][CH:22]=4)[OH:20])[CH2:17][CH2:18]3)=[CH:8][CH:7]=2)[CH2:3][CH2:2]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

4

反応物 2

HCID 6340IodoethaneHCID 53988844HCID 53988844、化合物

生成物 1

HCID 19063887N-[4-(cyclopropylmethoxy)phenylmethyl]-N-ethoxy-4-[bis(4-trifluoromethylphenyl)hydroxymethyl]-piperidinium iodide収率 40.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
0 °C

実験手順

A stirred mixture of 1.0 gram (0.002 mole) of N-[4-(cyclopropylmethoxy)phenylmethyl]-4-[bis(4-trifluoromethylphenyl)hydroxy-methyl]piperidine N-oxide, 0.3 gram (0.002 mole) of ethyl iodide, and about 5.0 mL of acetonitrile was heated at reflux for several hours. The reaction mixture was then cooled to 0° C., and petroleum ether was added. Upon completion of the addition the mixture was filtered and the filtrate was concentrated under reduced pressure, yielding 0.6 gram of N-[4-(cyclopropylmethoxy)phenylmethyl]-N-ethoxy-4-[bis(4-trifluoromethylphenyl)hydroxymethyl]-piperidinium iodide. The NMR spectrum was consistent with the proposed structure.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for several hours
  3. additionUpon completion of the addition the mixture
  4. filtrationwas filtered
  5. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-1189176dbe0e4db39aa581e346137e26
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05795901

反応ノート

読み込み中…

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