Piperazine → HCID 178517383, 화합물

HRID 330847노트

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HRID 330847 반응식
[OH-:1].[K+].[N:3]1([C:8]2[C:17]3[C:12](=[N:13][C:14](Cl)=[C:15]([Cl:18])[N:16]=3)[N:11]=[C:10](Cl)[N:9]=2)[CH2:7][CH2:6][CH2:5][CH2:4]1.[NH:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>O.O1CCCC1>[Cl:18][C:15]1[N:16]=[C:17]2[C:12](=[N:13][C:14]=1[OH:1])[N:11]=[C:10]([N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)[N:9]=[C:8]2[N:3]1[CH2:7][CH2:6][CH2:5][CH2:4]1

참가 물질

6

반응물 3

HCID 4837PiperazineHCID 14797Potassium HydroxideHCID 137998844-Pyrrolidin-1-yl-2,6,7-trichloropteridine

생성물 1

HCID 178517383HCID 178517383, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

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온도
-10 °C

실험 절차

a)+b) 460 μl (0.82 mmol) of a 10% solution of potassium hydroxide in water is added dropwise to a solution of 250 mg (0.82 mmol) 4-pyrrolidin-1-yl-2,6,7-trichloro-pteridine in 15 ml of tetrahydrofuran cooled to −10° C. The mixture is stirred for one hour at −10° C., slowly allowed to come up to ambient temperature and stirred for approx. another 16 hours. Then a solution of 318 mg (3.69 mmol) piperazine in 10 ml of tetrahydrofuran is added and the mixture is refluxed for approx. 16 hours. Then the solvent is eliminated in vacuo, the residue is mixed with water and extracted with dichloromethane. The organic phase is dried on sodium sulphate and the solvent is eliminated in vacuo. The residue is purified by chromatography. Yield 50 mg (14% of theoretical)

후처리

  1. customto come up to ambient temperature
  2. stirringstirred
  3. waitfor approx. another 16 hours
  4. temperaturethe mixture is refluxed for approx. 16 hours
  5. extractionextracted with dichloromethane
  6. customThe organic phase is dried on sodium sulphate
  7. customThe residue is purified by chromatography

출처 및 근거

ORD 기록
ord-328cd6c9d5bf4080855c6d50cf864177
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877756B2

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