Triphenylphosphine → 4-(4-Acryloyloxybutyloxy)-3-methyl-4'-phenylazo-azobenzene

HRID 28316

반응식

HRID 28316 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[N:9][C:10]2[CH:15]=[CH:14][C:13]([N:16]=[N:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:12][CH:11]=2)=[CH:4][C:3]=1[CH3:24].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[CH2:45][CH2:46][CH2:47][CH2:48][O:49][C:50](=[O:53])[CH:51]=[CH2:52].N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[C:50]([O:49][CH2:48][CH2:47][CH2:46][CH2:45][O:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[N:9][C:10]2[CH:15]=[CH:14][C:13]([N:16]=[N:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:12][CH:11]=2)=[CH:4][C:3]=1[CH3:24])(=[O:53])[CH:51]=[CH2:52]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 22736Disperse Yellow 7HCID 755884-Hydroxybutyl acrylateHCID 220568ethyl N-ethoxycarbonyliminocarbamate

생성물 1

HCID 178385924-(4-Acryloyloxybutyloxy)-3-methyl-4'-phenylazo-azobenzene

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-30 °C

실험 절차

To a solution of 0.63 g of 4-hydroxy-3-methyl4′-phenylazo-azobenzene, 1.05 g of triphenylphosphine and 0.58 g of 4-hydroxybutylacrylate in 10 ml THF; which was cooled to −30° C., was added dropwise a solution of 0.70 g of diethyl azodicarboxylate in 5 ml THF. After complete addition, the reaction mixture was stirred for further 45 min at room temperature, and then concentrated to dryness. The obtained yellow-red residue was purified by filtration on silica using methylenechloride as the eluent to give 0.65 g of pure yellow-orange crystalys; λmax. (CB 483): 395 nm.

후처리

  1. additionAfter complete addition
  2. concentrationconcentrated to dryness
  3. filtrationThe obtained yellow-red residue was purified by filtration on silica
  4. customto give 0.65 g of pure yellow-orange crystalys

출처 및 근거

ORD 기록
ord-7b03299eb0ab4ce5adf307e56e52b766
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07419620B2

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