반응식
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[C:5]([N:11]=[N:12][C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]=2[N+:21]([O-])=O)[C:4]=1[OH:24].[OH-].[Na+].C(S(O)=O)(N)=N.Cl>O.C(O)C>[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[C:5]([N:11]2[N:12]=[C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:14]3=[N:21]2)[C:4]=1[OH:24]참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 80 °C
실험 절차
In a 500 ml round bottom 3-neck flask equipped with a magnetic stirrer, addition funnel, powder addition funnel, and nitrogen inlet was added 2-(hydroxymethyl)-4-methoxy-6-((4-methoxy-2-nitrophenyl)diazenyl)phenol from Example 11 and 200 ml absolute ethanol (Pharmco Products, Brookfield, Conn.). NaOH pellets, 97% (Aldrich, 16.8 g, 420 mmol) were dissolved in 80 ml deionized water and approximately one-fourth of the solution was added dropwise to the azo mixture. The reaction mixture was heated to 80° C. and 22.6 g (209 mmol) formamidinesulfinic acid (Aldrich) and the remaining NaOH solution were added concurrently to the azo mixture over 0.5 hr. The mixture was heated at 80° C. for 3 hours, poured into 3.5 L water, and acidified to pH 4-5 with conc. HCl (J.T. Baker). The crude product was recrystallised from ethanol and then collected and vacuum dried (0.1 mm Hg) at 50° C. for 72 hours to give 7 g (27%) of a light yellow solid.
후처리
- customIn a 500 ml round bottom 3-neck flask equipped with a magnetic stirrer, addition funnel, powder addition funnel, and nitrogen inlet
- temperatureThe mixture was heated at 80° C. for 3 hours
- customThe crude product was recrystallised from ethanol
- customcollected
- customvacuum dried (0.1 mm Hg) at 50° C. for 72 hours
출처 및 근거
- ORD 기록
- ord-524ac225df2b4d2592ae68f22d1fa525
- 출처 데이터셋
- uspto-grants-2012_07
- 특허 번호
- US08232326B2
연결된 노트
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