Potassium Carbonate → HCID 16778897, 화합물

HRID 334521노트

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HRID 334521 반응식
ClC1C=C(C=C(Cl)C=1)C(NN)=O.[Cl:13][C:14]1[CH:15]=[C:16]([CH:25]=[C:26]([Cl:28])[CH:27]=1)[C:17]([NH:19][NH:20][C:21](=[O:24])[CH2:22][Cl:23])=O.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:23][CH2:22][C:21]1[O:24][C:17]([C:16]2[CH:15]=[C:14]([Cl:13])[CH:27]=[C:26]([Cl:28])[CH:25]=2)=[N:19][N:20]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 27359663,5-dichlorobenzohydrazideHCID 13365860HCID 13365860, 화합물

생성물 1

HCID 16778897HCID 16778897, 화합물수율 69.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

A mixture of compound 5 (700 mg, 2.14 mmol), compound 6 (222 mg, 1.86 mmol) and K2CO3 (772 mg, 5.59 mmol, 2 eq.) in 10 ml of DMF was heated to 100° C. for 3 hours. The reaction mixture was brought to ambient temperature, filtered and the filtrate was evaporated to obtain a crude residue which was purified by column chromatography using EtOAc/hexane (50:50) as an eluent to obtain compound 7 as a colorless liquid (340 mg). Yield: 50%.

후처리

  1. customwas brought to ambient temperature
  2. filtrationfiltered
  3. customthe filtrate was evaporated
  4. customto obtain a crude residue which
  5. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-1092bc6835c04968a7e0e0bc79cae3ab
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883827B2

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