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Trifluoroacetic acid → HCID 9888078, 화합물

HRID 723326
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HRID 723326 반응식
CO[CH:3](OC)[CH2:4][N:5]([C:21]1[CH:26]=[CH:25][C:24](OC2C=CC=CC=2)=[CH:23][CH:22]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])=[CH:11][CH:10]=1)=[O:7].F[C:37](F)(F)[C:38]([OH:40])=O>>[CH3:19][N:18]([CH3:20])[CH2:17][CH2:16][O:15][C:12]1[CH:11]=[CH:10][C:9]([N:8]2[CH:3]=[CH:4][N:5]([C:21]3[CH:26]=[CH:25][C:24]([O:40][C:38]4[CH:37]=[CH:11][CH:10]=[CH:9][CH:14]=4)=[CH:23][CH:22]=3)[C:6]2=[O:7])=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 21873333HCID 21873333, 화합물

생성물 1

HCID 9888078HCID 9888078, 화합물

실험 절차

1-(2,2-Dimethoxyethyl)-3-[4-(2-dimethylaminoethoxy)phenyl]-1-(4-phenoxy-phenyl)urea (0.33 g) was shaken with trifluoroacetic acid (5 ml) for 16 hours. Volatiles were removed and the residue was taken up in dichloromethane (10 ml) and washed with sodium hydroxide solution (0.1N; 1 ml). The aqueous phase was extracted with dichloromethane (10 ml), and the combined organic phases were concentrated. The residue was purified by chromatography on silica gel (eluent: dichloromethane/methanol 98:2 with 1% v/v 7N ammonia solution in methanol). The product with the molecular weight of 415.50 (C25H25N3O3); MS (ESI): 416 ([M+H]+), was obtained in this way.

후처리

  1. customVolatiles were removed
  2. washwashed with sodium hydroxide solution (0.1N; 1 ml)
  3. extractionThe aqueous phase was extracted with dichloromethane (10 ml)
  • concentrationthe combined organic phases were concentrated
  • customThe residue was purified by chromatography on silica gel (eluent
  • customMS (ESI): 416 ([M+H]+), was obtained in this way
  • 출처 및 근거

    ORD 기록
    ord-bde9c62aaa9d46c4b3f850ce716c244d
    출처 데이터셋
    uspto-grants-2006_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07141561B2

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