Cesium carbonate → 4-(2-Cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)benzenamine

HRID 1951285ノート

反応式

HRID 1951285 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([SH:14])=[CH:10][CH:9]=1.Cl[C:16]1[N:21]2[N:22]=[C:23]([CH:25]3[CH2:27][CH2:26]3)[CH:24]=[C:20]2[N:19]=[CH:18][CH:17]=1>CN(C=O)C.CCOC(C)=O>[CH:25]1([C:23]2[CH:24]=[C:20]3[N:19]=[CH:18][CH:17]=[C:16]([S:14][C:11]4[CH:12]=[CH:13][C:8]([NH2:7])=[CH:9][CH:10]=4)[N:21]3[N:22]=2)[CH2:27][CH2:26]1

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 145104-AminothiophenolHCID 846651637-Chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidine

生成物 1

HCID 670171844-(2-Cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)benzenamine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

To a mixture of cesium carbonate (0.606 g, 1.86 mmol) and 4-aminobenzenethiol (116 mg, 0.930 mmol) in DMF (3 mL) at RT was added 7-chloro-2-cyclopropylpyrazolo[1,5-a]pyrimidine (0.180 g, 0.930 mmol). The mixture was heated to 60° C. After 2 hrs the mixture was cooled to RT, diluted with EtOAc, and washed with water and brine. After drying the organic fraction with sodium sulfate, the solvent was removed in vacuo to afford 4-(2-cyclopropylpyrazolo[1,5-a]pyrimidin-7-ylthio)benzenamine, which was advanced without further purification. MS: Found M+H+=283.1.

後処理

  1. temperatureAfter 2 hrs the mixture was cooled to RT
  2. washwashed with water and brine
  3. dry with materialAfter drying the organic fraction with sodium sulfate
  4. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-e443de74d4154c86a94499e9f2b0afeb
出典データセット
uspto-grants-2013_03
特許番号
US08404694B2

反応ノート

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