Thiophosgene → 2,4-Dichloro-5-isothiocyanatopyridine

HRID 1177513노트

반응식

HRID 1177513 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 866387192,4-Dichloro-5-isothiocyanatopyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-539069a83c114ca393b26939ec82fbf7
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842685B2

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