Lawesson's reagent → HCID 59176770、化合物

HRID 215968ノート

反応式

HRID 215968 の反応式
[C:1]1([CH2:11][CH:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][C:13]2=O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:31]2)=CC=1>C1(C)C=CC=CC=1.CO>[C:1]1([CH2:11][CH:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][C:13]2=[S:31])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 2

HCID 87949Lawesson's reagentHCID 59176789HCID 59176789、化合物

生成物 1

HCID 59176770HCID 59176770、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒

反応条件

温度
160 °C

実験手順

A suspension of 200 mg (0.73 mmol) of 3-naphthalen-1-ylmethyl-imidazo[1,2-a]pyridin-2-one and 250 mg (0.62 mmol) of 2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane 2,4-disulfide (Lawesson's reagent) in 20 mL of toluene is heated at 160° C. for 1 h under microwave condition. The resulting mixture is dissolved in methanol and absorbed on silica gel. The slurry is dried under reduced pressure and is purified by flash chromatography on silica gel. The compound is eluted 5˜10% methanol in dichloromethane solution to give the desired compound.

後処理

  1. customabsorbed on silica gel
  2. customThe slurry is dried under reduced pressure
  3. customis purified by flash chromatography on silica gel
  4. washThe compound is eluted 5˜10% methanol in dichloromethane solution

出典と根拠

ORDレコード
ord-4afb7a9cdde94e8aafa4522f74e0360b
出典データセット
uspto-grants-2012_06
特許番号
US08193214B2

反応ノート

読み込み中…