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

HRID 349545
ノート
印刷プレビュー

反応式

HRID 349545 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 5235Sodium FluorideHCID 17961964HCID 17961964、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 179619914-Aminomethyl-1-propyl-5-tritylaminopyrazole収率 81.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2dde7729a76648eba2e1253a4f79fc1d
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179801B2

反応ノート

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