Water → HCID 19603718、化合物

HRID 1604656ノート

反応式

HRID 1604656 の反応式
[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]

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 22184407Ethyl 2-(iodomethyl)benzoateHCID 178441405HCID 178441405、化合物

生成物 2

HCID 19603718HCID 19603718、化合物HCID 19603742HCID 19603742、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-4cfc9535bbff483fbee11661b3f6c195
出典データセット
uspto-grants-1999_11
特許番号
US05994378

反応ノート

読み込み中…