Ethyl Acetate → HCID 68276344、化合物

HRID 1048756ノート

反応式

HRID 1048756 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[I:12][C:13]1[C:14]([O:23][CH3:24])=[N:15][C:16]([S:21][CH3:22])=[C:17]([CH:20]=1)[C:18]#[N:19].C(OCC)(=O)C>ClCCl>[I:12][C:13]1[C:14]([O:23][CH3:24])=[N:15][C:16]([S:21]([CH3:22])=[O:9])=[C:17]([CH:20]=1)[C:18]#[N:19]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 70297m-Chloroperbenzoic acidHCID 68276426HCID 68276426、化合物

生成物 1

HCID 68276344HCID 68276344、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.42 g (1.1 eq) of 70% 3-chloroperbenzoic acid is added to a solution of 1.6 g (5.23 mmol) of 5-iodo-6-methoxy-2-(methylthio)nicotinonitrile in 20 ml of dichloromethane. The reaction medium is stirred at room temperature for 1 hour. Ethyl acetate is added and the organic phase is washed with saturated sodium bicarbonate solution, dried on magnesium sulfate, filtered and evaporated to yield 1.63 g (97%) of 5-iodo-6-methoxy-2-(methylsulfinyl)nicotinonitrile in the form of a white powder which may also contain 5-iodo-6-methoxy-2-(methylsulfonyl)nicotinonitrile in small proportions (<20%). If necessary, the mixture is used as-is in the following steps.

後処理

  1. washthe organic phase is washed with saturated sodium bicarbonate solution
  2. customdried on magnesium sulfate
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-bfb2fe505a1846829e545151829cc070
出典データセット
uspto-grants-2016_07
特許番号
US09381195B2

反応ノート

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