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Tin tetrachloride → (2-Benzyl-4,5-dimethyl-thiophen-3-yl)-(4-methoxy-3,5-dimethyl-phenyl)-methanone

HRID 1954261
ノート
印刷プレビュー

反応式

HRID 1954261 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([CH3:13])[C:10]=1[O:11][CH3:12])[C:5]([OH:7])=O.C(Cl)(=O)C(Cl)=O.[CH3:20][C:21]1[S:22][C:23]([CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[CH:24][C:25]=1[CH3:26].[Sn](Cl)(Cl)(Cl)Cl>C(Cl)Cl.CN(C)C=O>[CH2:27]([C:23]1[S:22][C:21]([CH3:20])=[C:25]([CH3:26])[C:24]=1[C:5]([C:4]1[CH:8]=[C:9]([CH3:13])[C:10]([O:11][CH3:12])=[C:2]([CH3:1])[CH:3]=1)=[O:7])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=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

7

反応物 4

HCID 24287Tin tetrachlorideHCID 65578Oxalyl chlorideHCID 889443,5-Dimethyl-p-anisic acidHCID 102419632,3-Dimethyl-5-benzylthiophene

生成物 1

HCID 18430702(2-Benzyl-4,5-dimethyl-thiophen-3-yl)-(4-methoxy-3,5-dimethyl-phenyl)-methanone収率 82%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
触媒
HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

To a suspension of 3,5-dimethyl-p-anisic acid (15.2 g, 84.4 mmol, RN-21553-46-8) in anhydrous methylene chloride (200 mL) at room temperature under nitrogen was added oxalyl chloride (9.6 mL, 110 mmol) and N,N-dimethylformamide (5 drops). After two hours the solvent was removed. The resulting residue was dissolved in anhydrous methylene chloride (200 mL), and added to 2,3-dimethyl-5-benzylthiophene (17.1 g, 84.4 mmol) under nitrogen. The resulting mixture was, cooled to -78° C., and tin(IV) chloride (10.8 mL, 92.8 mmol) was added quickly. The -78° C. bath was removed and the mixture was stirred at room temperature for 2 h. The reaction mixture was then poured onto ice water (1 L), and the resulting mixture was extracted once with diethyl ether (700 mL), and a second time with diethyl ether (400 mL). The combined diethyl ether extracts were washed with ice water(500 mL), dilute sodium bicarbonate (500 mL), water (500 mL), brine (1L), and then dried (Na2SO4). Concentration under reduced pressure gave the title compound as a yellow oil (25.2 g, 82%): NMR (DMSO-d6) δ 7.40 (s, 2 H), 7.24-7.15 (m, 3 H), 7.06 (d, 2 H), 3.83 (s, 2 H), 3.70 (s, 3 H), 2.28 (s, 3 H), 2.26 (s, 6 H), 1.83 (s, 3 H).

後処理

  1. customAfter two hours the solvent was removed
  2. dissolutionThe resulting residue was dissolved in anhydrous methylene chloride (200 mL)
  3. customThe -78° C. bath was removed
  4. additionThe reaction mixture was then poured onto ice water (1 L)
  5. extractionthe resulting mixture was extracted once with diethyl ether (700 mL)
  6. washThe combined diethyl ether extracts were washed with ice water(500 mL), dilute sodium bicarbonate (500 mL), water (500 mL), brine (1L)
  7. dry with materialdried (Na2SO4)
  8. concentrationConcentration under reduced pressure

出典と根拠

ORDレコード
ord-170f002d6ffc4c32af24d3d9b30091bd
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06121271

反応ノート

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