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Ammonia → HCID 67388580, 화합물

HRID 269846
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HRID 269846 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]([NH2:31])([CH3:30])[CH3:29].C(N(C(C)C)CC)(C)C.S([O-])(O)=O.[Na+].N>O.CC(N(C)C)=O>[O:24]1[CH2:25][CH2:26][N:21]([CH2:20][C:17]2[CH:18]=[CH:19][C:14]([NH:13][C:6]3[N:5]=[C:4]([NH:31][CH:28]([CH3:30])[CH3:29])[C:9]([C:10]([NH2:12])=[O:11])=[CH:8][N:7]=3)=[CH:15][CH:16]=2)[CH2:22][CH2:23]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 222AmmoniaHCID 6363IsopropylamineHCID 81531DiisopropylethylamineHCID 23665763Sodium BisulfiteHCID 86602004HCID 86602004, 화합물

생성물 1

HCID 67388580HCID 67388580, 화합물

시약·촉매·용매 2

HCID 962
Water
용매
HCID 31374Dimethylacetamide용매

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온도
80 °C

실험 절차

A mixture of 450 mg of 4-methylsulfinyl-2-({4-[(N-oxidomorpholin -4-yl)methyl]phenyl}amino)pyrimidine-5-carboxamide, 0.29 ml of isopropylamine, 0.24 ml of diisopropylethylamine and 5 ml of DMA was stirred at 80° C. for 3 hours. The reaction mixture was cooled down to room temperature, mixed with 8 ml of 5% sodium hydrogen sulfite, followed by stirring for 1 hour. The reaction mixture was adjusted to pH 9 by adding 0.5 ml of concentrated aqueous ammonia, diluted with water and then extracted with chloroform. The organic layer was washed with saturated brine, and then the solvent was evaporated. The resulting residue was purified by a silica gel column chromatography (chloroform:methanol:aqueous ammonia), and the resulting pale brown oil was crystallized from ethyl acetate to obtain 50 mg of 2-{[4-(morpholinomethyl)phenyl]amino}-4-(2-propylamino)pyrimidine-5-carboxamide as colorless crystals.

후처리

  1. temperatureThe reaction mixture was cooled down to room temperature
  2. stirringby stirring for 1 hour
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with saturated brine
  5. customthe solvent was evaporated
  6. customThe resulting residue was purified by a silica gel column chromatography (chloroform:methanol:aqueous ammonia)
  7. customthe resulting pale brown oil was crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-8bc8a8a2ba9d4e7cb93236d7e4535dc4
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07449456B2

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