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N-(1,1-Dimethylethyl)benzenemethanamine → N-benzyl-t-butylamine hydrobromide

HRID 544751
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반응식

HRID 544751 반응식
C(NC(OC1C=C(C(=O)C[Br:21])C=C(OC(=O)NCC)C=1)=O)C.[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CC(C)=O>[BrH:21].[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
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참가 물질

4

반응물 2

HCID 76908N-(1,1-Dimethylethyl)benzenemethanamineHCID 204586013',5'-bis-(N-ethylcarbamoyloxy)-2-bromo acetophenone

생성물 1

HCID 20458608N-benzyl-t-butylamine hydrobromide수율 78.3%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of 8.0 g of 3',5'-bis-(N-ethylcarbamoyloxy)-2-bromo acetophenone in 100 ml of acetone was added 7.0 g of N-benzyl-t-butylamine. The mixture was refluxed for 18 hours. The 4.1 g of N-benzyl-t-butylamine hydrobromide formed and precipitated during the reaction was filtered off and the filtrate was acidified with conc. HCl. The filtrate was now evaporated to dryness and the title compound was isolated by column chromatography on Silica gel 60 using (1) CHCl3 /ethanol (2:1), (2) ethanol as eluants. The title compound was eluted in the ethanol fraction and recrystallized from ethanol/diethylether. The identity of the product was confirmed with NMR.

후처리

  1. temperatureThe mixture was refluxed for 18 hours

출처 및 근거

ORD 기록
ord-7fe92459100740a0b008c2a568a04930
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04451663

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