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Water → 4-Aminomethyl-1-propyl-5-tritylaminopyrazole

HRID 349545
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HRID 349545 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:10]1[C:14]([NH:15][C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:13]([C:35]#[N:36])[CH:12]=[N:11]1)[CH2:8][CH3:9].[F-].[Na+].O>O1CCCC1>[NH2:36][CH2:35][C:13]1[CH:12]=[N:11][N:10]([CH2:7][CH2:8][CH3:9])[C:14]=1[NH:15][C:16]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 5235Sodium FluorideHCID 17961964HCID 17961964, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 179619914-Aminomethyl-1-propyl-5-tritylaminopyrazole수율 81.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

To a suspension of lithium aluminum hydride (8.94 g) in tetrahydrofuran (600 ml) was added 1-propyl-5-tritylamino-1H-pyrazole-4-carbonitrile (37 g) at room temperature. The mixture was refluxed for 7 days. After cooling on an ice bath, sodium fluoride (40 g) and water (17 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. To the filtrate was added ethyl formate, and the mixture was refluxed for 24 hours. After evaporation of the solvent in vacuo, the residue was triturated with diisopropyl ether and dried in vacuo to give 4-aminomethyl-1-propyl-5-tritylaminopyrazole (30.3 g).

후처리

  1. temperatureThe mixture was refluxed for 7 days
  2. temperatureAfter cooling on an ice bath
  3. customThe insoluble materials were removed by filtration
  4. additionTo the filtrate was added ethyl formate
  5. temperaturethe mixture was refluxed for 24 hours
  6. customAfter evaporation of the solvent in vacuo
  7. customthe residue was triturated with diisopropyl ether
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-2dde7729a76648eba2e1253a4f79fc1d
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07179801B2

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