Triethylamine → 2-(4-Cyano-2-pyridyl)-4H-1,3-benzothiazine-4-one

HRID 499397노트

반응식

HRID 499397 반응식
[C:1]([O:10]C)(=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[SH:4].[C:12]([C:14]1[CH:19]=[C:18]([C:20]#[N:21])[CH:17]=[CH:16][N:15]=1)#[N:13].C(N(CC)CC)C>C1(C)C=CC=CC=1>[C:20]([C:18]1[CH:17]=[CH:16][N:15]=[C:14]([C:12]2[S:4][C:3]3[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=3[C:1](=[O:10])[N:13]=2)[CH:19]=1)#[N:21]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 21009Benzoic acid, 2-mercapto-, methyl esterHCID 1201442,4-Pyridinedicarbonitrile

생성물 1

HCID 597504122-(4-Cyano-2-pyridyl)-4H-1,3-benzothiazine-4-one수율 53%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of methyl thiosalicylate (0.65 g, 3.9 mmol), 2,4-dicyanopyridine (0.50 g, 3.9 mmol), triethylamine (0.81 ml, 5.8 mmol) and toluene (2.0 ml) was refluxed for 2.5 hrs. After cooling, the precipitated crystals were collected by filtration and recrystallized from acetone-chloroform to give the titled compound (0.54 g, 53%).

후처리

  1. temperaturewas refluxed for 2.5 hrs
  2. temperatureAfter cooling
  3. filtrationthe precipitated crystals were collected by filtration
  4. customrecrystallized from acetone-chloroform

출처 및 근거

ORD 기록
ord-18b82590e20a4bfe96d0243f401d17bd
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767665B2

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