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Azetidine → azetidin-1-yl(6,6-diphenyl-6,7-dihydro-1H-indazol-3-yl)methanone

HRID 1243824
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HRID 1243824 반응식
O.O[N:3]1[C:7]2C=CC=[CH:11][C:6]=2N=N1.Cl.CN(C)CCCN=C=NCC.[C:24]1([C:30]2([C:42]3[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=3)[CH2:38][C:37]3[NH:36][N:35]=[C:34]([C:39](O)=[O:40])[C:33]=3[CH:32]=[CH:31]2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.N1CCC1>ClCCl.C(N(CC)CC)C>[N:3]1([C:39]([C:34]2[C:33]3[CH:32]=[CH:31][C:30]([C:42]4[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=4)([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[CH2:38][C:37]=3[NH:36][N:35]=2)=[O:40])[CH2:11][CH2:6][CH2:7]1
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참가 물질

7

반응물 4

HCID 10422AzetidineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 219286736,6-diphenyl-6,7-dihydro-1H-indazole-3-carboxylic acid

생성물 1

HCID 21928925azetidin-1-yl(6,6-diphenyl-6,7-dihydro-1H-indazol-3-yl)methanone수율 65.9%

시약·촉매·용매 2

HCID 6344Dichloromethane용매3회HCID 8471Triethylamine용매

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온도
20 °C

실험 절차

0.256 g of 1-hydroxybenzotriazole hydrate and 0.364 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride are added to 0.5 g of 6,6-diphenyl-6,7-dihydro-1H-indazole-3-carboxylic acid in suspension in 100 cm3 of dichloromethane. After stirring for 30 minutes at a temperature in the region of 20° C., a solution of 0.114 g of azetidine and 0.303 g of triethylamine in 10 cm3 of dichloromethane is added to the reaction mixture. After stirring at a temperature in the region of 20° C. for about 20 hours, the reaction mixture is diluted with 300 cm3 of dichloromethane and then washed with 3 times 100 cm3 of water. The resulting organic phase is dried over magnesium sulphate, filtered and then concentrated to dryness under reduced pressure (13 kPa). The residue is purified by flash chromatography on a column of silica [eluent: dichloromethane/methanol (95/5 by volume)] to give 0.37 g of azetidin-1-yl(6,6-diphenyl-6,7-dihydro-1H-indazol-3-yl)methanone, in the form of a white powder, the characteristics of which are as follows:

후처리

  1. stirringAfter stirring at a temperature in the region of 20° C. for about 20 hours
  2. washwashed with 3 times 100 cm3 of water
  3. dry with materialThe resulting organic phase is dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated to dryness under reduced pressure (13 kPa)
  6. customThe residue is purified by flash chromatography on a column of silica [eluent: dichloromethane/methanol (95/5 by volume)]

출처 및 근거

ORD 기록
ord-bb89df7d39384d82b5675e4e64bf4332
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07119115B2

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