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Sodium Bicarbonate → HCID 18681037, 화합물

HRID 1276882
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HRID 1276882 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:21])[C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:19])[CH3:18])=[C:12]([NH2:20])[CH:11]=1.Br[CH2:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]2[N:31]=[N:32][S:33][CH:34]=2)=[CH:26][CH:25]=1.C(=O)([O-])O.[Na+]>CO>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][NH:8][C:9](=[O:21])[C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:19])[CH3:18])=[C:12]([NH:20][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]3[N:31]=[N:32][S:33][CH:34]=3)=[CH:26][CH:25]=2)[CH:11]=1
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참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 27764544-(1,2,3-Thiadiazol-4-yl)benzyl bromideHCID 18315403HCID 18315403, 화합물

생성물 1

HCID 18681037HCID 18681037, 화합물수율 64.3%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
70 °C

실험 절차

A solution of 0.800 g of N-(2-pyridylmethyl)-4-acetylamino-3-aminobenzamide in 10 ml of methanol were added 1.08 g of 4-(4-bromomethylphenyl)-1,2,3-thiadiazole and 0.710 g of sodium hydrogencarbonate, and the mixture was stirred at 70° C. for 1 hour. The reaction solution was concentrated, and was purified through silica-gel column chromatography (eluent: a mixture of ethyl acetate and methanol at a ratio of 9:1) to give 0.830 g of N-(2-pyridylmethyl)-4-acetylamino-3-[4-(1,2,3-thiadiazol-4-yl)benzylamino]benzamide

후처리

  1. concentrationThe reaction solution was concentrated
  2. customwas purified through silica-gel column chromatography (eluent
  3. additiona mixture of ethyl acetate and methanol at a ratio of 9:1)

출처 및 근거

ORD 기록
ord-fd4f678d717a4a8e961767a8452644e1
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06166219

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