Triphenylphosphine → 4-(2-{[5-Bromo-2-({3-chloro-4-[(2-methylphenyl)carbonyl]phenyl}amino)benzyl]oxy}ethyl)morpholine-3,5-dione

HRID 1797328노트

반응식

HRID 1797328 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[CH3:23])=[O:16])=[C:11]([Cl:24])[CH:10]=2)=[C:4]([CH2:25][O:26][CH2:27][CH2:28]O)[CH:3]=1.[NH:30]1[C:35](=[O:36])[CH2:34][O:33][CH2:32][C:31]1=[O:37].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[CH3:23])=[O:16])=[C:11]([Cl:24])[CH:10]=2)=[C:4]([CH:3]=1)[CH2:25][O:26][CH2:27][CH2:28][N:30]1[C:35](=[O:36])[CH2:34][O:33][CH2:32][C:31]1=[O:37]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 364836Morpholine-3,5-dioneHCID 10227340[4-({4-Bromo-2-[(2-hydroxyethoxy)methyl]phenyl}amino)-2-chlorophenyl](2-methylphenyl)methanone

생성물 1

HCID 221745154-(2-{[5-Bromo-2-({3-chloro-4-[(2-methylphenyl)carbonyl]phenyl}amino)benzyl]oxy}ethyl)morpholine-3,5-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of Compound 158 (47 mg, 0.1 mmol), morpholine-3,5-dione (16 mg, 0.14 mmol) and triphenylphosphine (37 mg, 0.14 mmol) in THF (5 ml) was added diethyl azodicarboxylate solution (40% in toluene, 0.1 ml, 0.23 mmol) at RT. The reaction solution was stirred at the same temperature for 18 h and concentrated in vacuo. The residue was purified by chromatography (petroleum ether/ethyl acetate 1:1) to furnish the title compound, which was impure. The product was further purified by preparative TLC (petroleum ether/ethyl acetate 1:1) to give the pure title compound as yellow oil.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified by chromatography (petroleum ether/ethyl acetate 1:1)

출처 및 근거

ORD 기록
ord-a8655a3014d241c6a8f1431bd05bc02e
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07034015B2

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