Lawesson's reagent → HCID 15239087, 화합물

HRID 274733노트

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HRID 274733 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 15239087HCID 15239087, 화합물수율 60.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

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온도
100 °C

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-d14e3d4452914fc582196a69e89a15dc
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389669

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