Thionyl Chloride → 3-Chloropyridine-2-carbonyl chloride

HRID 1497693

반응식

HRID 1497693 반응식
[Cl:1][C:2]1[C:3]([C:8]([OH:10])=O)=[N:4][CH:5]=[CH:6][CH:7]=1.S(Cl)([Cl:13])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:3]([C:8]([Cl:13])=[O:10])=[N:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 8246323-Chloropyridine-2-carboxylic acid

생성물 1

HCID 450814973-Chloropyridine-2-carbonyl chloride

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
120 °C

실험 절차

To a suspension of 3-chloropicolinic acid (1.58 g, 10 mmol) in toluene (6 mL) was added an excess of thionyl chloride (9.52 g, 5.84 mL, 80.0 mmol) at room temperature under a nitrogen atmosphere. The resulting suspension was heated to 120° C. (oil bath temperature) and stirred for 20 h. Then, the solvent and excess of thionyl chloride were removed under vacuum and the residue was dissolved one more time in toluene and the solvent was removed again. The resulting residue was dried under high vacuum and used in the next step.

후처리

  1. customThen, the solvent and excess of thionyl chloride were removed under vacuum
  2. dissolutionthe residue was dissolved one more time in toluene
  3. customthe solvent was removed again
  4. customThe resulting residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-0c111a772a66422795d657a647f2ebe2
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09199987B2

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