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Ammonia → HCID 23071590, 화합물

HRID 269847
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HRID 269847 반응식
CS([C:4]1[C:9]([C:10]([NH2:12])=[O:11])=[CH:8][N:7]=[C:6]([NH:13][C:14]2[CH:19]=[CH:18][C:17]([CH2:20][N+:21]3([O-])[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)=[CH:16][CH:15]=2)[N:5]=1)=O.[CH:28]1([NH2:31])[CH2:30][CH2:29]1.C(N(C(C)C)CC)(C)C.S([O-])(O)=O.[Na+].N>C(Cl)(Cl)Cl>[CH:28]1([NH:31][C:4]2[C:9]([C:10]([NH2:12])=[O:11])=[CH:8][N:7]=[C:6]([NH:13][C:14]3[CH:19]=[CH:18][C:17]([CH2:20][N:21]4[CH2:26][CH2:25][O:24][CH2:23][CH2:22]4)=[CH:16][CH:15]=3)[N:5]=2)[CH2:30][CH2:29]1
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참가 물질

7

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HCID 222AmmoniaHCID 69828CyclopropylamineHCID 81531DiisopropylethylamineHCID 23665763Sodium BisulfiteHCID 86602004HCID 86602004, 화합물

생성물 1

HCID 23071590HCID 23071590, 화합물수율 23.6%

시약·촉매·용매 1

HCID 6212
Chloroform
용매

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온도
90 °C

실험 절차

A 1 ml portion of chloroform solution containing 11.7 mg of 4-methylsulfinyl-2-({4-[(N-oxidomorpholin-4-yl)methyl]phenyl}amino)pyrimidine-5-carboxamide was mixed with 5.1 mg of cyclopropylamine and 5.8 mg of diisopropylethylamine, followed by stirring at 90° C. for 15 hours. A 1 ml portion of aqueous solution containing 50 mg of sodium hydrogen sulfite was added to the reaction mixture, followed by stirring at room temperature for 4 hours. This was mixed with 0.1 ml of aqueous ammonia and extracted with 2 ml of chloroform. By evaporating the solvent under a reduced pressure and fractionating the residue by an HPLC (Wakosil-II 5C18AR, 0.1% HCOOH—H2O/MeOH=7/3−0/10), 2.6 mg of 4-cyclopropylamino-2-(4-morpholin -4-ylmethylphenylamino)-pyrimidine-5-carboxamide was obtained.

후처리

  1. additionwas added to the reaction mixture
  2. stirringby stirring at room temperature for 4 hours
  3. extractionextracted with 2 ml of chloroform
  4. customBy evaporating the solvent under a reduced pressure

출처 및 근거

ORD 기록
ord-800bd13932e541d5807c4bb352fdc869
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07449456B2

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