Water → HCID 86614295、化合物

HRID 2239935ノート

反応式

HRID 2239935 の反応式
[H-].[Na+].[CH:3]1([CH:9]([OH:14])[C:10]([F:13])([F:12])[F:11])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[NH2:15][C:16]1[N:21]=[C:20](Cl)[CH:19]=[C:18]([Cl:23])[N:17]=1.O>C1COCC1.C(OCC)(=O)C>[Cl:23][C:18]1[CH:19]=[C:20]([O:14][CH:9]([CH:3]2[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]2)[C:10]([F:12])([F:13])[F:11])[N:21]=[C:16]([NH2:15])[N:17]=1

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 655222-Amino-4,6-dichloropyrimidineHCID 109430921-Cyclohexyl-2,2,2-trifluoroethan-1-ol

生成物 1

HCID 86614295HCID 86614295、化合物収率 65.2%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

NaH (80 mg, 60%, 3.0 mmol) was added to the solution of 1-cyclohexyl-2,2,2-trifluoro-ethanol (182 mg, 1 mmol) in 10 ml of anhydrous THF, the mixture was stirred for 20 minutes, 2-amino-4,6-dichloro-pyrimidine (164 mg, 1 mmol) was added and then the reaction mixture was heated at 70° C. for 1 hour. After cooling, 5 ml water was added and ethyl acetate (20 ml) was used to extract the product. The organic layer was dried over sodium sulfate. The solvent was removed by rotovap to give 202 mg of 4-chloro-6-[1-cyclohexyl-2,2,2-trifluoro-ethoxy]-pyrimidin-2-ylamine, yield 65%.

後処理

  1. temperatureAfter cooling
  2. extractionto extract the product
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. customThe solvent was removed by rotovap

出典と根拠

ORDレコード
ord-f3c3375aabe44bb8829764ea6af2a8f2
出典データセット
uspto-grants-2010_05
特許番号
US07723345B2

反応ノート

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