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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
ノート
印刷プレビュー

反応式

HRID 871863 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 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}carbamate収率 20%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
120 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-ab8b98b3ed4a42bd93a1638d7a2007b1
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08975250B2

反応ノート

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