Hydrogen Sulfide → Isothiazolo(3,4-b)pyridin-3-amine

HRID 2200508ノート

反応式

HRID 2200508 の反応式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[SH2:10]>N1C=CC=CC=1>[N:1]1[S:10][C:8]([NH2:9])=[C:7]2[CH:6]=[CH:5][CH:4]=[N:3][C:2]=12

参加物

4

反応物 2

HCID 402Hydrogen SulfideHCID 8182592-Amino-3-cyanopyridine

生成物 1

HCID 297118Isothiazolo(3,4-b)pyridin-3-amine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 2-amino-3-cyanopyridine (1.00 g, 8.40 mmol) in pyridine (8 mL) and TEA (0.8 mL) in a sealed tube, H2S gas was bubbled through for 5 min. It was then stirred at room temperature for 20 h. The mixture was concentrated in vacuo to dryness. The residue was dissolved in MeOH (10 mL). To the solution, aq. H2O2 (30%, 3 mL) was added. The mixture was then stirred at room temperature for 5 h, during which time, solids precipitated out. The solids were collected by filtration, dried on vacuum to give isothiazolo[3,4-b]pyridin-3-amine (860 mg).

後処理

  1. concentrationThe mixture was concentrated in vacuo to dryness
  2. dissolutionThe residue was dissolved in MeOH (10 mL)
  3. additionTo the solution, aq. H2O2 (30%, 3 mL) was added
  4. stirringThe mixture was then stirred at room temperature for 5 h, during which time, solids
  5. customprecipitated out
  6. filtrationThe solids were collected by filtration
  7. customdried on vacuum

出典と根拠

ORDレコード
ord-2f774f56a30a40818cef199a5c98e94d
出典データセット
uspto-grants-2016_06
特許番号
US09359308B2

反応ノート

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