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Dimethylformamide → Methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate

HRID 1604648
ノート
印刷プレビュー

反応式

HRID 1604648 の反応式
[C]=O.FC(F)(F)S(O[C:9]1[CH:10]=[CH:11][C:12]2[O:16][C:15]([C:17]3[S:18][CH:19]=[C:20]([C:22]([CH3:25])([CH3:24])[CH3:23])[N:21]=3)=[CH:14][C:13]=2[CH:26]=1)(=O)=O.C1(OP(CCCP([O:57][C:58]2C=CC=CC=2)(OC2C=CC=CC=2)=O)(OC2C=CC=CC=2)=O)C=CC=CC=1.C(N(CC)CC)C.CN(C)[CH:73]=[O:74]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.CO>[C:22]([C:20]1[N:21]=[C:17]([C:15]2[O:16][C:12]3[CH:11]=[CH:10][C:9]([C:73]([O:57][CH3:58])=[O:74])=[CH:26][C:13]=3[CH:14]=2)[S:18][CH:19]=1)([CH3:25])([CH3:24])[CH3:23]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 196036842-(4-Tert-butylthiazol-2-yl)benzofuran-5-yl trifluoromethanesulfonateHCID 538511551,3-Bis(diphenylphosphono)propaneHCID 178418416HCID 178418416、化合物

生成物 1

HCID 19603836Methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

Carbon monoxide was introduced by bubbling to a mixture of 2-(4-tert-butylthiazol-2-yl)benzofuran-5-yl trifluoromethanesulfonate (6.0 g), palladium acetate (99.7 mg), 1,3-bis(diphenylphosphono)propane (183 mg, 0.44 mmol) and triethylamine (4.13 ml) in a mixed solvent of methanol (15 ml) and N,N-dimethylformamide (30 ml) at room temperature for 1 hour. The mixture was warmed to 70° C. and stirred under carbon monoxide balloon for 3 hours. The resulting mixture was filtered through celite and the residue was washed with ethyl acetate. The filtrate and washing solution was combined and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using ethyl acetate-n-hexane as eluent to give methyl 2-(4-tert-butylthiazol-2-yl)benzofuran-5-carboxylate (3.92 g) as a colorless powder.

後処理

  1. filtrationThe resulting mixture was filtered through celite
  2. washthe residue was washed with ethyl acetate
  3. washThe filtrate and washing solution
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-438352edabd341d88dfbc1795d420f22
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05994378

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート