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Sulfur Dioxide → Lithium 4-methyl-3-thiophenesulfinate

HRID 434591
ノート
印刷プレビュー

反応式

HRID 434591 の反応式
Br[C:2]1[C:6]([CH3:7])=[CH:5][S:4][CH:3]=1.C([Li:12])CCC.[S:13](=[O:15])=[O:14]>C(OCC)C.CCCCCC>[CH3:7][C:6]1[C:2]([S:13]([O-:15])=[O:14])=[CH:3][S:4][CH:5]=1.[Li+:12]
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 3

HCID 1119Sulfur DioxideHCID 27349353-Bromo-4-methylthiopheneHCID 178418339Butyllithium

生成物 1

HCID 23669555Lithium 4-methyl-3-thiophenesulfinate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

To 30 g of 3-bromo-4-methylthiophene in 150 ml of anhydrous ethyl ether under nitrogen at -70° to -75° C. was added, cautiously, during 30 minutes 111 ml of 1.6 M butyl lithium in hexane. The mixture was stirred for an additional thirty minutes and then 30 ml of liquified sulfur dioxide was added at such a rate that the temperature of the reaction mixture was maintained below -70° C. Upon completion of the addition, the mixture was stirred for an additional 90 minutes at -75° C. and then allowed to stand overnight at room temperature. The resulting precipitate was filtered and washed with ethyl ether, dried in air and in vacuo under nitrogen to yield 30 g of the desired salt, m.p. >250° C.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturewas maintained below -70° C
  2. additionUpon completion of the addition
  3. stirringthe mixture was stirred for an additional 90 minutes at -75° C.
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with ethyl ether
  6. customdried in air and in vacuo under nitrogen

出典と根拠

ORDレコード
ord-fa5d4458813a4b4c9bafc5a3632af464
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04398939

反応ノート

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