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Triethylamine → 2-(2'-Nitro-4'-methylsulfonylbenzoyl)-4-propargyl-1,3-cyclohexanedione

HRID 358543
ノート
印刷プレビュー

反応式

HRID 358543 の反応式
[CH2:1]([CH:4]1[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][C:5]1=[O:11])[C:2]#[CH:3].[CH3:12][S:13]([C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[C:18]([N+:25]([O-:27])=[O:26])[CH:17]=1)(=[O:15])=[O:14].C(N(CC)CC)C.[C-]#N.[K+].C1OCCOCCOCCOCCOCCOC1>C(#N)C>[N+:25]([C:18]1[CH:17]=[C:16]([S:13]([CH3:12])(=[O:15])=[O:14])[CH:24]=[CH:23][C:19]=1[C:20]([CH:6]1[C:5](=[O:11])[CH:4]([CH2:1][C:2]#[CH:3])[CH2:9][CH2:8][C:7]1=[O:10])=[O:21])([O-:27])=[O:26]
参加物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 8471TriethylamineHCID 9032Potassium CyanideHCID 2855718-Crown-6HCID 114805364-(Prop-2-yn-1-yl)cyclohexane-1,3-dioneHCID 148001864-(Methanesulfonyl)-2-nitrobenzoyl chloride

生成物 1

HCID 200662982-(2'-Nitro-4'-methylsulfonylbenzoyl)-4-propargyl-1,3-cyclohexanedione
収率 44.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4Propargyl-1,3-cyclohexanedione (3.75 g, 25 mmol) and 4-methanesulfonyl-2-nitrobenzoyl chloride (6.06 g, 23 mmol) were dissolved in acetonitrile (100 mL) at 0° C. Triethylamine (9.6 mL, 69 mmol) was added. The mixture was then stirred for 3 hours. To the mixture was then added potassium cyanide (5.0 g) and 18-crown-6 ether (0.5 g) in one portion. The mixture was stirred for 3 days. After dilution with ether, the solution was washed with 1N HC1 and extracted with 5% K2CO3. The basic extract was acidified with concentrated HC1 and extracted with diethyl ether. The ether extract was washed with brine, dried over MgSO4, and concentrated under vacuum, yielding 3.9 g of the desired product, an orange solid, m.p. 65-70° C. The structure was confirmed by nuclear magnetic spectroscopy, infrared spectroscopy, and mass spectroscopy.

後処理

  1. stirringThe mixture was stirred for 3 days
  2. washAfter dilution with ether, the solution was washed with 1N HC1
  3. extractionextracted with 5% K2CO3
  4. extractionThe basic extract
  5. extractionextracted with diethyl ether
  6. extractionThe ether extract
  7. washwas washed with brine
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-920785c218cf4fe790f3acaf11cbf2de
出典データセット
uspto-grants-1991_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04997473

反応ノート

読み込み中…

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