p-Toluenesulfonic acid → HCID 57691009、化合物

HRID 1511274ノート

反応式

HRID 1511274 の反応式
[C:1]1([C:7]2[CH:8]=[CH:9][C:10]3[N:11]([C:13]([CH2:16][NH:17][C:18]4[CH:23]=[CH:22][N:21]=[CH:20][C:19]=4[NH2:24])=[N:14][N:15]=3)[N:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:25](OCC)(OCC)OCC.CC1C=CC(S(O)(=O)=O)=CC=1>>[N:17]1([CH2:16][C:13]2[N:11]3[N:12]=[C:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)[CH:8]=[CH:9][C:10]3=[N:15][N:14]=2)[C:18]2[CH:23]=[CH:22][N:21]=[CH:20][C:19]=2[N:24]=[CH:25]1

参加物

4

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 31214Ethyl orthoformateHCID 67503473N4-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)pyridine-3,4-diamine

生成物 1

HCID 57691009HCID 57691009、化合物

反応条件

温度
60 °C

実験手順

A mixture of N4-((6-phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methyl)pyridine-3,4-diamine (0.0650 g, 0.20 mmol), triethyl orthoformate (5.0 ml, 30 mmol), and p-TsOH (0.0039 g, 0.020 mmol) was heated at 60° C. After 2 h reaction is complete. Reaction was concentrated. Took up in DMSO and purified on RPHPLC. Fractions containing product were treated with 91 sodium carbonate and volatiles removed. Collected product by filtration. MS m/z=328.1 [M+1]+. Calc'd for C18H13N7: 327.3.

後処理

  1. customAfter 2 h reaction
  2. customReaction
  3. concentrationwas concentrated
  4. custompurified on RPHPLC
  5. additionFractions containing product
  6. additionwere treated with 91 sodium carbonate and volatiles
  7. customremoved
  8. filtrationCollected product by filtration

出典と根拠

ORDレコード
ord-570e6b085fc54651a8a3dbd0f7270eff
出典データセット
uspto-grants-2012_07
特許番号
US08212041B2

反応ノート

読み込み中…