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Water → tert-Butyl {3-[7-amino-6-carbamoyl-2-(4-morpholin-4-ylphenylamino)-5-oxo-5H-pyrido[2,3-d]pyrimidin-8-yl]propyl}carbamate

HRID 871863
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HRID 871863 반응식
[C:1]([O:5][C:6](=[O:27])[NH:7][CH2:8][CH2:9][CH2:10][N:11]1[C:16]2[N:17]=[C:18](Cl)[N:19]=[CH:20][C:15]=2[C:14](=[O:22])[C:13]([C:23](=[O:25])[NH2:24])=[C:12]1[NH2:26])([CH3:4])([CH3:3])[CH3:2].[N:28]1([C:34]2[CH:39]=[CH:38][C:37]([NH2:40])=[CH:36][CH:35]=2)[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1.O.C([O-])(O)=O.[Na+]>CN1C(=O)CCC1>[NH2:26][C:12]1[N:11]([CH2:10][CH2:9][CH2:8][NH:7][C:6](=[O:27])[O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[C:16]2[N:17]=[C:18]([NH:40][C:37]3[CH:36]=[CH:35][C:34]([N:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[CH:39][CH:38]=3)[N:19]=[CH:20][C:15]=2[C:14](=[O:22])[C:13]=1[C:23](=[O:25])[NH2:24]
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참가 물질

6

반응물 4

HCID 962WaterHCID 75655Benzenamine, 4-(4-morpholinyl)-HCID 516892Sodium BicarbonateHCID 86673138tert-Butyl [3-(7-amino-6-carbamoyl-2-chloro-5-oxo-5H-pyrido[2,3-d]pyrimidin-8-yl)propyl]carbamate

생성물 1

HCID 67325689tert-Butyl {3-[7-amino-6-carbamoyl-2-(4-morpholin-4-ylphenylamino)-5-oxo-5H-pyrido[2,3-d]pyrimidin-8-yl]propyl}carbamate수율 20%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
120 °C

실험 절차

A mixture of 0.60 g (1.51 mmol) of the product prepared in step 11.3 and 0.53 g (3.02 mmol) of 4-morpholin-4-ylphenylamine in 6.5 mL of NMP is placed in a 10 mL microwave tube. The sealed tube is placed in the microwave oven (CEM machine, Discovery model) and the mixture is heated under pressure at 120°C. for 60 minutes at a power of 75 W, and then cooled to room temperature. 15 mL of water and then 5 mL of saturated aqueous NaHCO3 are added and the precipitate formed is drained by suction and then dried in an oven. The crude solid is triturated in methanol, drained by suction and dried in an oven under vacuum. 0.159 g of the expected product is obtained in solid form. Yield=20%.

후처리

  1. customis placed in a 10 mL microwave tube
  2. temperaturecooled to room temperature
  3. customthe precipitate formed
  4. customdried in an oven
  5. customThe crude solid is triturated in methanol
  6. customdried in an oven under vacuum

출처 및 근거

ORD 기록
ord-ab8b98b3ed4a42bd93a1638d7a2007b1
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975250B2

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