p-Toluenesulfonic acid → HCID 57691009, 화합물

HRID 1511274노트

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HRID 1511274 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 57691009HCID 57691009, 화합물

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-570e6b085fc54651a8a3dbd0f7270eff
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08212041B2

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