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Water → 4-(3-Aminopropyl)-1-(2-triphenylmethyloxyethyl)-5-aminopyrazole

HRID 349553
ノート
印刷プレビュー

反応式

HRID 349553 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7](/[CH:9]=[CH:10]/[C:11]1[CH:12]=[N:13][N:14]([CH2:17][CH2:18][O:19][C:20]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]=1[NH2:16])#[N:8].[F-].[Na+].O>O1CCCC1>[NH2:8][CH2:7][CH2:9][CH2:10][C:11]1[CH:12]=[N:13][N:14]([CH2:17][CH2:18][O:19][C:20]([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)([C:27]2[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:15]=1[NH2:16]
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 179619694-[(E)-2-cyanoethenyl]-1-[2-(trityloxy)ethyl]-5-aminopyrazoleHCID 21226445Aluminium lithium hydride

生成物 1

HCID 179619934-(3-Aminopropyl)-1-(2-triphenylmethyloxyethyl)-5-aminopyrazole収率 90%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

To a suspension of lithium aluminum hydride (5.41 g) in tetrahydrofuran (200 ml) was added a solution of 4-[(E)-2-cyanoethenyl]-1-[2-(trityloxy)ethyl]-5-aminopyrazole (15 g) in tetrahydrofuran (100 ml) under ice-cooling. The mixture was refluxed for 3.5 hours. After cooling on an ice bath, sodium fluoride (24 g) and water (10.3 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. The filtrate was concentrated in vacuo to give 4-(3-aminopropyl)-1-(2-triphenylmethyloxyethyl)-5-aminopyrazole (13.7 g). This product was used in the next step without further purification.

後処理

  1. temperaturecooling
  2. temperatureThe mixture was refluxed for 3.5 hours
  3. temperatureAfter cooling on an ice bath
  4. customThe insoluble materials were removed by filtration
  5. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-f466e2e378d24b20abc8830681963482
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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