Thiophosgene → 2,6-Dichloro-3-isothiocyanatopyridine

HRID 1177389ノート

反応式

HRID 1177389 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[Cl:7][C:8]1[C:13]([NH2:14])=[CH:12][CH:11]=[C:10]([Cl:15])[N:9]=1.[C:16](Cl)(Cl)=[S:17]>C(Cl)Cl>[Cl:7][C:8]1[C:13]([N:14]=[C:16]=[S:17])=[CH:12][CH:11]=[C:10]([Cl:15])[N:9]=1

参加物

5

反応物 3

HCID 10040ThiophosgeneHCID 10340Sodium CarbonateHCID 1128462,6-Dichloro-3-pyridylamine

生成物 1

HCID 715192602,6-Dichloro-3-isothiocyanatopyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A slurry of sodium carbonate (15.2 g, 144 mmol), 2,6-dichloropyridin-3-amine (9.00 g, 55.2 mmol), and thiophosgene (5.50 mL, 71.8 mmol) in 100 mL anhydrous DCM was allowed to stir in a sealed vessel for 2 days. The reaction mixture was filtered through a glass frit, rinsing with DCM. The filtrate was concentrated in vacuo to give 2,6-dichloro-3-isothiocyanatopyridine as a peach-colored solid.

後処理

  1. filtrationThe reaction mixture was filtered through a glass frit
  2. washrinsing with DCM
  3. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-d88cd8ee7a4e4e9e8f167200188416fb
出典データセット
uspto-grants-2010_11
特許番号
US07842685B2

反応ノート

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