Trifluoroacetonitrile → HCID 178472209、化合物

HRID 542128ノート

反応式

HRID 542128 の反応式
[C:1]([CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])(=[O:4])[CH2:2][CH3:3].[Na].[F:12][C:13]([F:17])([F:16])[C:14]#[N:15]>COCCOC>[NH2:15]/[C:14](/[C:13]([F:17])([F:16])[F:12])=[C:5](/[C:1](=[O:4])[CH2:2][CH3:3])\[C:6]([O:8][CH2:9][CH3:10])=[O:7]

参加物

5

反応物 3

HCID 67710TrifluoroacetonitrileHCID 78656Ethyl 3-oxovalerateHCID 5360545Sodium2 回

生成物 1

HCID 178472209HCID 178472209、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a mechanically stirred solution of 287 g (1.99 mol) of ethyl propionylacetate in 500 ml of dry DME was added under nitrogen 8.6 g (0.348 mol) of freshly cut sodium. After all sodium had dissolved, 256 g (2.69 mol) of trifluoroacetonitrile was added over a 35 hour period. The reaction mixture was concentrated. The residue was washed with water and extracted into 500 ml of ether. The ether solution was dried and concentrated. The residue was kugelrohr distilled at 67 Pa. and then was redistilled at 67 Pa through a spinning band column. The first fraction (bp 40°-78° C.) was discarded. The next fraction (bp 79°-82° C.) was 151 g (31.6%) of product, nD25 1.4574.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. washThe residue was washed with water
  3. extractionextracted into 500 ml of ether
  4. dry with materialThe ether solution was dried
  5. concentrationconcentrated
  6. distillationThe residue was kugelrohr distilled at 67 Pa
  7. distillationand then was redistilled at 67 Pa through a spinning band column

出典と根拠

ORDレコード
ord-1252b550ae124bd5b158217c426e7714
出典データセット
uspto-grants-1987_04
特許番号
US04655816

反応ノート

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