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Hydrochloric Acid → methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate

HRID 1892507
ノート
印刷プレビュー

反応式

HRID 1892507 の反応式
[Cl-].[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH2:11][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[N:10]=1)(=[O:4])[CH3:3].CC(C)([O-])C.[K+].[CH:37]([C:39]1[CH:40]=[C:41](/[CH:44]=[CH:45]/[C:46]([O:48][CH3:49])=[O:47])[S:42][CH:43]=1)=O.Cl.[Cl-].[Na+]>CN(C)C=O>[C:2]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH:11]=[CH:37][C:39]2[CH:40]=[C:41](/[CH:44]=[CH:45]/[C:46]([O:48][CH3:49])=[O:47])[S:42][CH:43]=2)[N:10]=1)(=[O:4])[CH3:3]
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

7

反応物 5

HCID 313Hydrochloric AcidHCID 5234Sodium ChlorideHCID 23665647Potassium tert-butoxideHCID 86092822[(2-Acetylaminothiazol-4-yl)methyl](triphenyl)phosphonium chlorideHCID 86650009methyl (2E)-3-(4-formylthiophen-2-yl)acrylate

生成物 1

HCID 86650010
methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate
収率 82.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

To {[2-(acetylamino)-1,3-thiazol-4-yl]methyl}(triphenyl)phosphoniumchloride (6.602 g, 14.58 mmol) was added anhydrous N,N-dimethylformamide (30 ml), and the mixture was cooled to 0° C. Potassium tert-butoxide (3.146 g, 28.03 mmol) was added, and the mixture was stirred at 0° C. for 15 min. A solution of methyl (2E)-3-(4-formylthiophen-2-yl)acrylate (2.200 g, 11.21 mmol) in anhydrous N,N-dimethylformamide (30 ml) was added dropwise, and the mixture was stirred at 0° C. for 1 hr. The reaction mixture was poured into ice-cooled dil. hydrochloric acid (600 ml, containing 15 mmol as HCl). Sodium chloride (10 g) was added, and the mixture was extracted 3 times with ethyl acetate. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 500 g, ethyl acetate:hexane=1:1) to give methyl (2E)-3-(4-{2-[2-(acetylamino)-1,3-thiazol-4-yl]vinyl}thiophen-2-yl)acrylate (3.090 g, 9.241 mmol, 82.4%) as a yellowish-white solid.

後処理

  1. stirringthe mixture was stirred at 0° C. for 1 hr
  2. additionThe reaction mixture was poured into ice-
  3. extractionthe mixture was extracted 3 times with ethyl acetate
  4. washThe combined organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (FUJI SILYSIA CHEMICAL LTD. BW-300SP 500 g, ethyl acetate:hexane=1:1)

出典と根拠

ORDレコード
ord-4fe7580cdc7640609dcd1f89699e5378
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08507690B2

反応ノート

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