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3-Nitrophthalic anhydride → HCID 792947, 화합물

HRID 2301912
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인쇄 미리보기

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HRID 2301912 반응식
[N+:1]([C:4]1[CH:14]=[CH:13][CH:12]=[C:6]2[C:7]([O:9][C:10](=[O:11])[C:5]=12)=O)([O-:3])=[O:2].[CH3:15][C@@H:16]([NH2:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(Cl)(Cl)Cl>[C:17]1([C@H:16]([N:23]2[C:10](=[O:11])[C:5]3[C:6](=[CH:12][CH:13]=[CH:14][C:4]=3[N+:1]([O-:3])=[O:2])[C:7]2=[O:9])[CH3:15])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 216313-Nitrophthalic anhydrideHCID 6431891-Phenethylamine, (+)-

생성물 1

HCID 792947HCID 792947, 화합물수율 73%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
180 °C

실험 절차

386 mg of 3-nitrophthalic anhydride and 242 mg of (R)-α-methylbenzylamine were charged in an egg-plant type flask of 50 ml, followed by stirring under heating at a temperature of 180° C. for 1.5 hours. After cooled, the reaction product was dissolved in chloroform, purified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v), recrystallized from a mixed solvent of n-hexane-ethyl acetate, to obtain 430 mg of the desired product as a light yellow powder. Yield: 73%. m.p. 115-117° C.; MS(EI+) 296(M)+

후처리

  1. temperatureAfter cooled
  2. custompurified by silica gel column chromatography (eluent; methylene chloride:methanol=30:1 v/v)
  3. customrecrystallized from a mixed solvent of n-hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-a1fbca80a68742168f9738b613b55c2c
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06429212B1

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