Diethyl bromomalonate → diethyl N-benzyl-N-(2,4-dimethoxybenzyl)-amino-malonate

HRID 1388873노트

반응식

HRID 1388873 반응식
[CH2:1]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][C:11]=1[O:18][CH3:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH:21]([C:27]([O:29][CH2:30][CH3:31])=[O:28])[C:22]([O:24][CH2:25][CH3:26])=[O:23]>>[CH2:1]([N:8]([CH:21]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][C:11]=1[O:18][CH3:19])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

3

반응물 2

HCID 69637Diethyl bromomalonateHCID 784822Benzyl-(2,4-dimethoxy-benzyl)-amine

생성물 1

HCID 13422977diethyl N-benzyl-N-(2,4-dimethoxybenzyl)-amino-malonate수율 81%

실험 절차

The compound obtained in the step (1a), is converted into the corresponding base and 175 g (0.68 moles) of benzyl (2,4-dimethoxybenzyl)-amine obtained are stirred with 89.6 g (0.38 moles, 64 ml) of diethyl bromomalonate at room temperature until the reaction mixture solidifies. The solidified mixture is triturated with about one liter of ether and the crystalline precipitate is filtered off. (In this way the excess of the starting amine can be recovered as the hydrobromide with a yield of 95%). The filtrate is evaporated and the residual oil is triturated with ethanol. 114.5 g (81%) of diethyl N-benzyl-N-(2,4-dimethoxybenzyl)-amino-malonate are obtained, melting at 62° to 63° C. after crystallization from ethanol.

후처리

  1. customThe compound obtained in the step (1a)
  2. customobtained
  3. customThe solidified mixture is triturated with about one liter of ether
  4. filtrationthe crystalline precipitate is filtered off
  5. custom(In this way the excess of the starting amine can be recovered as the hydrobromide with a yield of 95%)
  6. customThe filtrate is evaporated
  7. customthe residual oil is triturated with ethanol

출처 및 근거

ORD 기록
ord-0611d698c1a14f70934c54682dfee80e
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04434099

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