Water → HCID 10135175、化合物

HRID 733013ノート

反応式

HRID 733013 の反応式
[NH2:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][N:7]2[C:11]3[N:12]=[C:13]([NH2:21])[N:14]=[C:15]([C:16]4[O:17][CH:18]=[CH:19][CH:20]=4)[C:10]=3[N:9]=[N:8]2)=[CH:4][C:3]=1[CH3:24].Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27].O>N1C=CC=CC=1>[NH2:21][C:13]1[N:14]=[C:15]([C:16]2[O:17][CH:18]=[CH:19][CH:20]=2)[C:10]2[N:9]=[N:8][N:7]([CH2:6][C:5]3[CH:22]=[CH:23][C:2]([NH:1][C:26](=[O:27])[O:28][CH2:29][CH3:30])=[C:3]([CH3:24])[CH:4]=3)[C:11]=2[N:12]=1

参加物

5

反応物 3

HCID 962WaterHCID 10928Ethyl chloroformateHCID 21874557Vipadenant

生成物 1

HCID 10135175HCID 10135175、化合物収率 100%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A suspension of 3-(4-amino-3-methylbenzyl)-7-(2-furyl)-3H-[1,2,3]triazolo[4,5-d]pyrimidine-5-amine (260 mg, 0.812 mmol) in pyridine (5 mL) at room temperature was treated dropwise with ethyl chloroformate (0.155 mL, 1.62 mmol), stirred for 30 min, poured into water (30 mL), extracted with EtOAc (2×10 mL) and the combined organic phase was dried (MgSO4) and concentrated in vacuo to give the title compound (318 mg, 100%) as a beige solid.

後処理

  1. extractionextracted with EtOAc (2×10 mL)
  2. dry with materialthe combined organic phase was dried (MgSO4)
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b2a62cf02a9e4db2a92c38577f22d551
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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