Pyridinium, 1-(2-ethoxy-2-oxoethyl)-, bromide (1:1) → N-(Ethoxycarbonylmethyl)pyridinium Tetraphenylborate

HRID 1614295ノート

反応式

HRID 1614295 の反応式
[Br-].[CH2:2]([O:4][C:5]([CH2:7][N+:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:6])[CH3:3].[C:14]1([B-:20]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Na+]>O>[C:33]1([B-:20]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1.[CH2:2]([O:4][C:5]([CH2:7][N+:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:6])[CH3:3]

参加物

4

反応物 2

HCID 87028Pyridinium, 1-(2-ethoxy-2-oxoethyl)-, bromide (1:1)HCID 2723787Sodium Tetraphenylborate

生成物 1

HCID 19432273N-(Ethoxycarbonylmethyl)pyridinium Tetraphenylborate収率 45.11%

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

To a solution of 24.61 grams (0.10 mol) of N-(ethoxycarbonylmethyl)pyridinium bromide in 100 milliliters of water, there was added a solution of 34.22 grams (0.10 mol) of sodium tetraphenylborate in 150 milliliters of water. The mixture was diluted with 1 liter of water and filtered. The solid collected was dissolved in methylene chloride, the water layer was separated and the organic layer was dried over MgSO4 and concentrated. Recrystallization from ethyl acetate yielded 21.9 grams of product (45.11% of theory); mp=150°-152° C.

後処理

  1. filtrationfiltered
  2. customThe solid collected
  3. dissolutionwas dissolved in methylene chloride
  4. customthe water layer was separated
  5. dry with materialthe organic layer was dried over MgSO4
  6. concentrationconcentrated
  7. customRecrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-1d4248cf4eca48c7a5a478a6817b58e0
出典データセット
uspto-grants-1993_03
特許番号
US05196538

反応ノート

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