Water → HCID 21874759、化合物

HRID 733014ノート

反応式

HRID 733014 の反応式
[NH2:1][C:2]1[N:3]=[C:4]([C:25]2[O:26][CH:27]=[CH:28][CH:29]=2)[C:5]2[N:10]=[N:9][N:8]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([NH:18][C:19](=O)[O:20]CC)=[C:14]([CH3:24])[CH:13]=3)[C:6]=2[N:7]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+].O>C1COCC1>[NH2:1][C:2]1[N:3]=[C:4]([C:25]2[O:26][CH:27]=[CH:28][CH:29]=2)[C:5]2[N:10]=[N:9][N:8]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([NH:18][CH:19]=[O:20])=[C:14]([CH3:24])[CH:13]=3)[C:6]=2[N:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 10135175HCID 10135175、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 21874759HCID 21874759、化合物収率 7.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of ethyl 4-((5-amino-7-(2-furyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine-3-yl)methyl)-2-methylphenylcarbamate (318 mg, 0.81 mmol) and LiAlH4 (62 mg, 1.62 mmol) in dry THF (30 mL) was refluxed overnight, cooled to room temperature, treated with 13% aqueous NaOH solution (0.1 mL) then water (0.3 mL), stirred for 30 min, filtered through Celite and concentrated in vacuo. The resulting solid was triturated with THF and filtered to give the title compound (20 mg, 7%) as a yellow solid.

後処理

  1. temperaturewas refluxed overnight
  2. filtrationfiltered through Celite
  3. concentrationconcentrated in vacuo
  4. customThe resulting solid was triturated with THF
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-2fe827aec1e74c818e3694ec75c1eb0c
出典データセット
uspto-grants-2009_09
特許番号
US07589097B2

反応ノート

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