Hydrochloric Acid → 1-Hydroxy-1-[4-[2-(5-phenyl-[1,2,4]-oxadiazol-3-yl)-ethoxy]-benzyl]-urea

HRID 22369

반응식

HRID 22369 반응식
[C:1]1([C:7]2[O:11][N:10]=[C:9]([CH2:12][CH2:13][O:14][C:15]3[CH:23]=[CH:22][C:18]([CH2:19][NH:20][OH:21])=[CH:17][CH:16]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C[Si]([N:28]=[C:29]=[O:30])(C)C.O.Cl>O1CCOCC1>[OH:21][N:20]([CH2:19][C:18]1[CH:17]=[CH:16][C:15]([O:14][CH2:13][CH2:12][C:9]2[N:8]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[O:11][N:10]=2)=[CH:23][CH:22]=1)[C:29]([NH2:28])=[O:30]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 70696Trimethylsilyl isocyanateHCID 10591115N-[4-[2-(5-phenyl-[1,2,4]-oxadiazol-3-yl)-ethoxy]-benzyl]-hydroxylamine

생성물 1

HCID 107131011-Hydroxy-1-[4-[2-(5-phenyl-[1,2,4]-oxadiazol-3-yl)-ethoxy]-benzyl]-urea수율 70%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of N-[4-[2-(5-phenyl-[1,2,4]-oxadiazol-3-yl)-ethoxy]-benzyl]-hydroxylamine (1.5 g, 4.82 mmol in dioxane (70 mL) was added trimethylsilylisocyanate (0.84 g, 7.23 mmol). After stirring for 2 hours at room temperature the mixture was poured into H2O, acidified with HCl (2N), and extracted with EtOAc. The organic extracts were dried over MgSO4. Evaporation and crystallization from acetone/ether (after cooling to 0° C.), gave a white solid (1.2 g, 70% yield, m.p. 135°-136° C.).

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe organic extracts were dried over MgSO4
  3. customEvaporation and crystallization from acetone/ether (after cooling to 0° C.)

출처 및 근거

ORD 기록
ord-cedd0dd128d9425ca8c717c3fc1015ca
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428048

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