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

HRID 1614295

반응식

HRID 1614295 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 19432273N-(Ethoxycarbonylmethyl)pyridinium Tetraphenylborate수율 45.11%

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d4248cf4eca48c7a5a478a6817b58e0
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05196538

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