Lawesson's reagent → HCID 15239087、化合物

HRID 1975394ノート

反応式

HRID 1975394 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([C:8]([NH2:10])=O)[NH:6][CH:7]=1)#[N:2].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:20]2)=CC=1>C1(C)C=CC=CC=1.O1CCCC1>[C:1]([C:3]1[CH:4]=[C:5]([C:8](=[S:20])[NH2:10])[NH:6][CH:7]=1)#[N:2]

参加物

5

反応物 2

HCID 87949Lawesson's reagentHCID 152390864-cyano-1H-pyrrole-2-carboxamide

生成物 1

HCID 15239087HCID 15239087、化合物収率 60.1%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
100 °C

実験手順

A mixture of 4-cyanopyrrole-2-carboxamide (1.35 g, 10.0 mmol) and 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (4.0 g, 9.9 mmol) in toluene is heated at 100° C. for 41/2 hours, diluted with tetrahydrofuran and heated at reflux for 20 minutes. The reaction mixture is then cooled and concentrated in vacuo to obtain a residue. Chromatography of the residue using silica gel and a 4:1 hexanes/ethyl acetate mixture gives the title product as a yellow solid (0.9 g, mp 253° C. dec.).

後処理

  1. temperatureheated
  2. temperatureat reflux for 20 minutes
  3. temperatureThe reaction mixture is then cooled
  4. concentrationconcentrated in vacuo
  5. customto obtain a residue

出典と根拠

ORDレコード
ord-c4b80ffb89b84f31b1466b3116379866
出典データセット
uspto-grants-1994_02
特許番号
US05286742

反応ノート

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