Water → HCID 19603718, 화합물

HRID 1604656노트

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HRID 1604656 반응식
[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([C:19]4[NH:23][N:22]=[N:21][N:20]=4)=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].I[CH2:25][C:26]1[CH:36]=[CH:35][CH:34]=[CH:33][C:27]=1[C:28]([O:30][CH2:31][CH3:32])=[O:29].C(=O)([O-])[O-].[K+].[K+].O>CC(=O)CC>[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([C:19]4[N:23]=[N:22][N:21]([CH2:25][C:26]5[CH:36]=[CH:35][CH:34]=[CH:33][C:27]=5[C:28]([O:30][CH2:31][CH3:32])=[O:29])[N:20]=4)=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3].[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([C:19]4[N:23]([CH2:25][C:26]5[CH:36]=[CH:35][CH:34]=[CH:33][C:27]=5[C:28]([O:30][CH2:31][CH3:32])=[O:29])[N:22]=[N:21][N:20]=4)=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 22184407Ethyl 2-(iodomethyl)benzoateHCID 178441405HCID 178441405, 화합물

생성물 2

HCID 19603718HCID 19603718, 화합물HCID 19603742HCID 19603742, 화합물

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 5-[2-(4-tert-butylthiazol-2-yl)benzofuran-5-yl]-1H-tetrazole (1.55 g), ethyl 2-iodomethylbenzoate (1.67 g) and potassium carbonate (1.80 g) in 2-butanone (15 ml) was stirred under reflux for 5 hours. After being cooled, the resulting mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with a mixture of toluene and ethyl acetate. The fractions containing object compound were combined and concentrated under reduced pressure to give 5-[2-(4-tert-butylthiazol-2-yl)benzofuran-5-yl]-2-[2-(ethoxycarbonyl)phenylmethyl]-2H-tetrazole (2.05 g) and 5-[2-(4-tert-butylthiazol-2-yl)benzofuran-5-yl]-1-[2-(ethoxycarbonyl)phenylmethyl]-1H-tetrazole (0.24 g).

후처리

  1. temperatureunder reflux for 5 hours
  2. temperatureAfter being cooled
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. washeluted with a mixture of toluene and ethyl acetate
  8. additionThe fractions containing object compound
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4cfc9535bbff483fbee11661b3f6c195
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05994378

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