2,6-Difluorobenzamide → 2,6-Difluorobenzene-1-carbothioamide

HRID 73597

反応式

HRID 73597 の反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([NH2:6])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4](=[S:21])[NH2:6]

参加物

4

反応物 2

HCID 874392,6-DifluorobenzamideHCID 87949Lawesson's reagent

生成物 1

HCID 126832122,6-Difluorobenzene-1-carbothioamide収率 99%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2, 6 difluorobenzamide (1 eq) and Lawesson's reagent (0.5 eq.) in toluene (0.2 M) was heated at 90° C. for 14 hours. Upon cooling the volatiles were removed in vacuo and purified by SiO2 chromatography (25% EtOAc/hexanes) yielding 2,6-difluorobenzothioamide as a light yellow solid (99%). LCMS (m/z): 174.1 (MH+); LC Rt=2.19 min.

後処理

  1. temperatureUpon cooling the volatiles
  2. customwere removed in vacuo
  3. custompurified by SiO2 chromatography (25% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-b0b6e2c6e1cd425cb1c695a43492eb1a
出典データセット
uspto-grants-2014_09
特許番号
US08829193B2

関連ノート

読み込み中…