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Homoveratrylamine → HCID 19814324, 화합물

HRID 466597
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HRID 466597 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH2:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[CH2:14]([N:21]1[CH2:32][CH2:31][C:24]2([O:28][C:27](=[O:29])[O:26][C:25]2=[CH2:30])[CH2:23][CH2:22]1)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>C1(C)C(C)=CC=CC=1.CCCCCCC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][N:13]2[C:25]([OH:26])([CH3:30])[C:24]3([CH2:23][CH2:22][N:21]([CH2:14][C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH2:32][CH2:31]3)[O:28][C:27]2=[O:29])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 8421HomoveratrylamineHCID 19814218HCID 19814218, 화합물

생성물 1

HCID 19814324HCID 19814324, 화합물수율 94%

시약·촉매·용매 2

HCID 7237O-Xylene용매HCID 8900Heptane용매

실험 절차

19.9 g of 2-(3,4-dimethoxyphenyl)ethylamine are portionwise added to a solution of 25.9 g of 8-benzyl-4-methylene-2-oxo-1,3-dioxa-8-azaspiro[4,5]decane in 35 ml of anhydrous xylene under stirring. Meanwhile the temperature of the reaction mixture increases to 35° to 40° C. The reaction mixture is left to stand at room temperature overnight, then the crystalline reaction mixture is diluted with n-heptane and filtered. The solid precipitate obtained is recrystallized from ethanol to obtain the title compound in 94% yield, m.p.: 181°-183° C.

후처리

  1. temperatureMeanwhile the temperature of the reaction mixture increases to 35° to 40° C
  2. waitThe reaction mixture is left
  3. filtrationfiltered
  4. customThe solid precipitate obtained
  5. customis recrystallized from ethanol

출처 및 근거

ORD 기록
ord-eeeabe2351f34092821d1da0836cc939
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05157038

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