Water → HCID 69583568、化合物

HRID 1743531ノート

反応式

HRID 1743531 の反応式
[I-].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([CH2:12][N+:13]3([CH2:18][CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[OH2:20]>>[OH-:20].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([CH2:12][N+:13]3([CH2:18][CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:10][CH2:11]2)=[CH:5][CH:4]=1

参加物

3

反応物 2

HCID 962WaterHCID 695836481-{[1-(4-Chlorophenyl)cyclopropyl]methyl}-1-ethylpyrrolidin-1-ium iodide

生成物 1

HCID 69583568HCID 69583568、化合物収率 96%

実験手順

The hydroxide form of 1-[1-(4-chloro-phenyl)-cyclopropylmethyl]-1-ethyl-pyrrolidinium cation is obtained by an ion exchange treatment of the iodide salt with Ion-Exchange Resin-OH (BIO RAD® AH1-X8). In a 1-liter volume plastic bottle, 100 gm (255 mmol) of 1-[1-(4-chloro-phenyl)-cyclopropylmethyl]-1-ethyl-pyrrolidinium iodide is dissolved in 300 ml de-ionized water. Then, 320 gm of the ion exchange resin is added and the solution is allowed to gently stir overnight. The mixture is then filtered, and the resin cake is rinsed with minimal amount of de-ionized water. The filtrate is analyzed for hydroxide concentration by titration analysis on a small sample of the solution with 0.1N HCl. The reaction yields 96% of (245 mmol) of the desired 1-[1-(4-chloro-phenyl)-cyclopropylmethyl]-1-ethyl-pyrrolidinium hydroxide (hydroxide concentration of 0.6 M).

後処理

  1. filtrationThe mixture is then filtered
  2. washthe resin cake is rinsed with minimal amount of de-ionized water
  3. concentrationThe filtrate is analyzed for hydroxide concentration by titration analysis on a small sample of the solution with 0.1N HCl

出典と根拠

ORDレコード
ord-f5dda04eccdf42659759c513bec4487a
出典データセット
uspto-grants-2006_03
特許番号
US07011811B2

反応ノート

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