Thiophosgene → 2,4-Dichloro-5-isothiocyanatopyridine

HRID 1177513ノート

反応式

HRID 1177513 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][C:3]=1[NH2:9].C(=O)([O-])[O-].[Na+].[Na+].[C:16](Cl)(Cl)=[S:17]>C(Cl)Cl>[Cl:8][C:6]1[CH:7]=[C:2]([Cl:1])[C:3]([N:9]=[C:16]=[S:17])=[CH:4][N:5]=1

参加物

5

反応物 3

HCID 10040ThiophosgeneHCID 10340Sodium CarbonateHCID 5957294,6-Dichloropyridin-3-amine

生成物 1

HCID 866387192,4-Dichloro-5-isothiocyanatopyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirring slurry of 4,6-dichloropyridin-3-amine (2.00 g, 12 mmol) and sodium carbonate (3.4 g, 32 mmol) in 10 mL DCM was added thiophosgene (1.2 mL, 16 mmol). The orange mixture was sealed and allowed to stir at ambient temperature overnight. The reaction mixture was filtered, rinsing with DCM, and the filtrate concentrated in vacuo to give 2,4-dichloro-5-isothiocyanatopyridine as an orange solid. MS (ESD m/z: calculated: 203.9; Observed: 204.9 (M++1).

後処理

  1. customThe orange mixture was sealed
  2. filtrationThe reaction mixture was filtered
  3. washrinsing with DCM
  4. concentrationthe filtrate concentrated in vacuo

出典と根拠

ORDレコード
ord-539069a83c114ca393b26939ec82fbf7
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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