Triethylamine → 6-Methoxy-2-pyridinecarbonitrile

To an ice cold solution of 6-methoxy-pyridine-2-carboxylic acid amide (300 mg, 1.97 mmol) in THF (3 mL) were added triethylamine (1.25 mL, 8.68 mmol) and dropwise added TFAA (0.61 mL, 4.34 mmol). The reaction mixture was allowed to warm to room temperature and stirred overnight. The volatiles were concentrated in vacuo and the liquid residue was added dropwise to a vigorously stirred, ice cold, pH 7 phosphate buffer solution (5 mL). After 15 min of further stirring the yellowish solid was filtered and air dried for 1 h to yield 250 mg (95%) of 6-methoxy-pyridine-2-carbonitrile as yellowish solid, m/z 135.4 [M+1]+.

1. concentrationThe volatiles were concentrated in vacuo
2. additionthe liquid residue was added dropwise to
3. stirringa vigorously stirred
4. stirringAfter 15 min of further stirring the yellowish solid
5. filtrationwas filtered
6. customair dried for 1 h

ORD 기록

ord-1163420d0764436bbedaf7dba524e5f4

출처 데이터셋

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08552205B2