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

HRID 1951285노트

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HRID 1951285 반응식
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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e443de74d4154c86a94499e9f2b0afeb
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404694B2

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