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Tetrahydrofuran → (+) (2aS,4R)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indol

HRID 5425
ノート
印刷プレビュー

反応式

HRID 5425 の反応式
C([N:20]1[C:28]2[CH:27]=[CH:26][C:25](C#N)=[C:24]3[CH2:31][CH:32]([N:34]([CH2:38][CH2:39][CH3:40])[CH2:35][CH2:36][CH3:37])[CH2:33][CH:22]([C:23]=23)[CH2:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C[Mg]Br.[NH4+].[Cl-].C1C[O:49][CH2:48][CH2:47]1>C(OCC)C>[C:48]([C:25]1[CH:26]=[CH:27][C:28]2[NH:20][CH2:21][C@H:22]3[CH2:33][C@@H:32]([N:34]([CH2:38][CH2:39][CH3:40])[CH2:35][CH2:36][CH3:37])[CH2:31][C:24]=1[C:23]=23)(=[O:49])[CH3:47]
参加物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 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 19069121(+)-1-Trityl-6-cyano-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indoleHCID 178418573HCID 178418573、化合物

生成物 1

HCID 18652841(+) (2aS,4R)-6-acetyl-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indol

試薬・触媒・溶媒 1

HCID 3283
Diethyl Ether
溶媒

実験手順

A solution of 2.4 g (4.6 mmol) (+)-1-trityl-6-cyano-4-(di-n-propylamino)-1,2,2a,3,4,5-hexahydrobenz[cd]indole in 100 mL of THF was treated with 25 mL of 2.0M methylmagnesium bromide in diethyl ether. The reaction mixture was refluxed for 16 hr. The reaction mixture was cooled and excess Grignard reagent was decomposed with addition of saturated NH4Cl solution. The reaction mixture was extracted with ethyl acetate. The organic solution was evaporated to an oil. The oil was dissolved in 25 mL of 5N HCl and the solution was stirred at room temperature for 30 min. The acidic solution was made alkaline with the addition of excess concentrated NH4OH solution. The basic mixture was extracted twice with ethyl acetate. The combined organic solution was washed once with saturated NaCl solution and dried over MgSO4. The ethyl acetate solution was evaporated to yield 1.4 g of an oil. Chromatography of this oil over silicia gel with ethyl acetate as eluent gave 1.2 g (87%) of product. Recrystallization from hexanes yielded 840 mg of the product (+) ketone.

後処理

  1. temperatureThe reaction mixture was refluxed for 16 hr
  2. temperatureThe reaction mixture was cooled
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. customThe organic solution was evaporated to an oil
  5. dissolutionThe oil was dissolved in 25 mL of 5N HCl
  6. additionwith the addition of excess concentrated NH4OH solution
  7. extractionThe basic mixture was extracted twice with ethyl acetate
  8. washThe combined organic solution was washed once with saturated NaCl solution
  9. dry with materialdried over MgSO4
  10. customThe ethyl acetate solution was evaporated

出典と根拠

ORDレコード
ord-42b89d4ecc9c4ad3a03f64ca5c2ac1f8
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05244911

反応ノート

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