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3-[3-(2H-Benzotriazol-2-yl)-4-hydroxyphenyl]propyl 2-methyl-2-propenoate → HCID 21708848, 화합물

HRID 651552
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HRID 651552 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][O:11][C:12](=[O:16])[C:13]([CH3:15])=[CH2:14])=[CH:4][C:3]=1[N:17]1[N:21]=[C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]2=[N:18]1.[CH3:26][O-:27].[Na+].CO>C1(C)C(C)=CC=CC=1>[N:18]1[N:17]([C:3]2[C:2]([OH:1])=[C:7]([CH2:2][C:7]3[CH:6]=[C:5]([CH3:8])[CH:4]=[C:3]([N:17]4[N:18]=[C:19]5[CH:25]=[CH:24][CH:23]=[CH:22][C:20]5=[N:21]4)[C:26]=3[OH:27])[CH:6]=[C:5]([CH2:8][CH2:9][CH2:10][O:11][C:12](=[O:16])[C:13]([CH3:15])=[CH2:14])[CH:4]=2)[N:21]=[C:20]2[CH:22]=[CH:23][CH:24]=[CH:25][C:19]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 220350653-[3-(2H-Benzotriazol-2-yl)-4-hydroxyphenyl]propyl 2-methyl-2-propenoateHCID 23694274Sodium methanolate methanol

생성물 1

HCID 21708848HCID 21708848, 화합물수율 71%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Ten grams (30.9 mmols) of crude 2-(3′-N,N-diethylaminomethyl-2′-hydroxy-5′-methylphenyl)-2H-benzotriazole obtained following the procedures of Synthesis Example 1 and 10.5 g (31.1 mmols) of 2-(2′-hydroxy-5′-methacryloyloxypropylphenyl)-2H-benzotriazole were dissolved in 64 ml of xylene, and 1.5 ml of a 28% sodium methylate•methanol solution were added thereto. The mixture was then refluxed in a nitrogen stream for 10 hours. After the completion of the reaction, the reaction mixture was cooled to room temperature. Yellow crystals precipitated at this point were separated through filtration, and recrystallized from chloroform to obtain 12.8 g of 6-(2H-benzotriazol-2-yl)-4-methacryloyloxypropyl-2-[3′-(2H-benzotriazol-2-yl)-2′-hydroxy-5′-methylphenyl]methylphenol (hereinafter abbreviated as “RUVA-3”) as white crystals (yield 71.0%, purity 98.6%).

후처리

  1. temperatureThe mixture was then refluxed in a nitrogen stream for 10 hours
  2. customAfter the completion of the reaction
  3. customYellow crystals precipitated at this point
  4. customwere separated through filtration
  5. customrecrystallized from chloroform

출처 및 근거

ORD 기록
ord-8345c004bde04e5b950804e3579c53bf
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06281313B1

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