Benzenesulfonyl cyanide → 2-Benzenesulfonyl-5-chloropyridine

HRID 1953795

反応式

HRID 1953795 の反応式
C(O[CH:5]=[C:6]([Cl:9])[CH:7]=[CH2:8])(=O)C.[C:10]1([S:16]([C:19]#[N:20])(=[O:18])=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C1(C)C=CC=CC=1>[C:10]1([S:16]([C:19]2[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][N:20]=2)(=[O:17])=[O:18])[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

参加物

4

反応物 2

HCID 10313279Benzenesulfonyl cyanideHCID 542547732-Chloro-1,3-butadienyl acetate

生成物 1

HCID 101989402-Benzenesulfonyl-5-chloropyridine収率 90.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

A tubular reactor (capacity:1 ml, voidage:100%) was heated to 100° C. To the reactor was fed a toluene solution of 2-chloro-1,3-butadienyl acetate (44 volume percent, 3.0 moles/L) at a flow rate of 6.4 ml/hour, and benzenesulfonyl cyanide (79 volume percent, 4.69 moles/L) at a flow rate of 4.1 ml/minute for 1 hour (residence time 5.7 minutes). The effluent was ice-cooled for recrystallization, the crystals were collected by filtration, washed with cold toluene and dried under reduced pressure using a vacuum pump to give 4.39 g of 2-benzenesulfonyl-5-chloropyridine (yield 90.1%).

後処理

  1. customfor 1 hour
  2. custom(residence time 5.7 minutes)
  3. temperaturecooled for recrystallization
  4. filtrationthe crystals were collected by filtration
  5. washwashed with cold toluene
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-f7dad87f3dd9430488f110fdfe4b9bf2
出典データセット
uspto-grants-2000_09
特許番号
US06118005

関連ノート

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