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Hydrochloric Acid → 2-(1-Benzenesulfonyl-1H-pyrrol-3-yl)-1-(2,3-difluoro-phenyl)-ethanone

HRID 2249513
ノート
印刷プレビュー

反応式

HRID 2249513 の反応式
[C:1]1([S:7]([N:10]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([OH:18])=O)=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Li]N([Si](C)(C)C)[Si](C)(C)C.COC(=O)[C:32]1[CH:37]=[CH:36][CH:35]=[C:34]([F:38])[C:33]=1[F:39].Cl>C1COCC1>[C:1]1([S:7]([N:10]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([C:32]3[CH:37]=[CH:36][CH:35]=[C:34]([F:38])[C:33]=3[F:39])=[O:18])=[CH:11]2)(=[O:8])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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

6

反応物 4

HCID 313Hydrochloric AcidHCID 2782927Methyl 2,3-difluorobenzoateHCID 13157056(1-Benzenesulfonyl-1H-pyrrol-3-yl)-acetic acidHCID 178418261HCID 178418261、化合物

生成物 1

HCID 692886012-(1-Benzenesulfonyl-1H-pyrrol-3-yl)-1-(2,3-difluoro-phenyl)-ethanone収率 62.1%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
0 °C

実験手順

To a solution of (1-benzenesulfonyl-1H-pyrrol-3-yl)-acetic acid (1.3 g, 4.90 mmol) in THF was added LiN(TMS)2 (12 mL, 1.0M in THF, 12 mmol) at −78° C. The resulting solution was stirred at this temperature for 1 hour and 0° C. for 1 hour and then was cooled to −78° C. again. To this solution was added 2,3-difluoro-benzoic acid methyl ester (1.1 g, 6.40 mmol) and the reaction was stirred at room temperature for 14 hours. The solution was poured into 2N HCl and extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered, and evaporated. The crude product was purified by flash column eluting with 20% of EtOAc in hexanes to afford the title compound as a yellow oil (1.1 g, 58%). 1H NMR (500 MHz, CDCl3) δ7.77 (d, 2H), 7.50 (m, 2H), 7.42 (t, 2H), 7.28 (m, 1H), 7.05 (m, 3H), 6.18 (m, 1H), 3.98 (s, 2H) ppm. MS (ES+): m/e=362.1 (M+H); LC/Method A/3.98 min.

後処理

  1. temperaturewas cooled to −78° C. again
  2. stirringthe reaction was stirred at room temperature for 14 hours
  3. extractionextracted with EtOAc
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude product was purified by flash column
  8. washeluting with 20% of EtOAc in hexanes

出典と根拠

ORDレコード
ord-d14bddca6d8e4c64a4c4f8930f0d7837
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314885B2

反応ノート

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