Ammonia → HCID 67195016、化合物

HRID 2401328ノート

反応式

HRID 2401328 の反応式
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([O:10][C:11]2[N:12]([CH2:26][CH2:27][CH3:28])[C:13](=[O:25])[C:14]3[NH:15][C:16]([CH:20]4[CH2:24][CH2:23][CH2:22][CH2:21]4)=[N:17][C:18]=3[N:19]=2)[CH:5]=1.C[N:31]1CCCN2C1=NCCC2.N>C1COCC1>[CH:20]1([C:16]2[NH:15][C:14]3[C:13](=[O:25])[N:12]([CH2:26][CH2:27][CH3:28])[C:11]([O:10][C:6]4[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=4)[C:3]([NH2:31])=[O:2])=[N:19][C:18]=3[N:17]=2)[CH2:21][CH2:22][CH2:23][CH2:24]1

参加物

5

反応物 3

HCID 222AmmoniaHCID 1235837-Methyl-1,5,7-triazabicyclo[4.4.0]dec-5-eneHCID 52933921HCID 52933921、化合物

生成物 1

HCID 67195016HCID 67195016、化合物収率 61.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 3-(8-Cyclopentyl-6-oxo-1-propyl-6,7-dihydro-1H-purin-2-yloxy)-benzoic acid methyl ester (0.07 g, 0.17 mmol, 1.0 eq) and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene (0.034 g, 0.247 m·mol, 1.4 eq) was taken in THF. To this was added Liq.NH3 (˜3 g) through septum in sealed tube at −78° C. and then heated at 50° C. overnight. Crude reaction mixture was purified by preparative TLC to give the product as a white solid (0.04 g) in 60% yield.

後処理

  1. additionTo this was added Liq
  2. customCrude reaction mixture
  3. customwas purified by preparative TLC

出典と根拠

ORDレコード
ord-38944f2a34de42068966ba0c6b776e95
出典データセット
uspto-grants-2014_08
特許番号
US08796290B2

反応ノート

読み込み中…