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Ethylenediamine → HCID 86739113, 화합물

HRID 2295365
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HRID 2295365 반응식
O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[C:13]12[C:26](=[O:27])[O:25][C:23](=O)[C:14]=1[CH2:15][CH2:16][C:17]1[C:22]2=[CH:21][CH:20]=[CH:19][CH:18]=1.[CH2:28]([NH2:31])[CH2:29][NH2:30]>C1(C)C=CC=CC=1>[NH2:30][CH2:29][CH2:28][N:31]1[C:23](=[O:25])[C:14]2[CH2:15][CH2:16][C:17]3[C:22]([C:13]=2[C:26]1=[O:27])=[CH:21][CH:20]=[CH:19][CH:18]=3
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3301EthylenediamineHCID 1422143,4-Dihydro-1,2-naphthalenedicarboxylic anhydrideHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 86739113HCID 86739113, 화합물수율 97.8%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
60 °C

실험 절차

27.6 g of toluene-p-sulphonic acid monohydrate are added to a solution of 27.62 g (0.138 mol) of 3,4-dihydronaphthalene-1,2-dicarboxylic acid anhydride in 300 ml of toluene, followed by 8.69 g of ethylenediamine. The mixture is heated to 60° C. for 30 minutes and then refluxed for 30 minutes, removing continuously the toluene and the water as they are formed by destillation. The residue is dried under vacuo to yield 32.7 g (90.0% of theory) of N-(2'-aminoethyl)-3,4-dihydronaphthalene-1,2-dicarboximide in the form of its toluene-p-sulphonic acid salt. This salt may be purified by recrystallisation from toluene.

후처리

  1. temperaturerefluxed for 30 minutes
  2. customremoving continuously the toluene
  3. customthe water as they are formed by destillation
  4. customThe residue is dried under vacuo

출처 및 근거

ORD 기록
ord-6fabce03e14c4113947d1613b70a98e8
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04424366

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