Trifluoroacetic acid → 4-Chloro-5-iodo-2-methoxypyridine
反応式
[Cl:1][C:2]1[C:7]([I:8])=[CH:6][N:5]=[C:4](N)[CH:3]=1.[C:10](O)(C(F)(F)F)=[O:11].N(OC(C)(C)C)=O>CO>[Cl:1][C:2]1[C:7]([I:8])=[CH:6][N:5]=[C:4]([O:11][CH3:10])[CH:3]=1参加物
5
実験手順
To a solution of 4-chloro-5-iodo-pyridin-2-ylamine (64.2 g, 0.25 mol) in methanol (1.1 L) and TFA (93.7 mL, 1.26 mol) was added tert-butyl nitrite (150 mL, 1.26 mol) so as to maintain temperature less than 3° C. The resultant mixture was stirred at RT for 1 h then allowed to warm to RT and stirred for 16 h. The reaction was quenched by the careful addition of water then concentrated in vacuo to ¼ volume. The resultant residue was treated with water (1 L) and the precipitate formed collected by filtration and dried in vacuo at 35° C. to give the title compound (62.3 g, 92%). Contains 16% impurity. 1H NMR 400 MHz (DMSO-d) δ: 8.56 (1 H, s), 7.20 (1 H, s), 3.86 (3 H, s).
後処理
- temperatureto maintain temperature less than 3° C
- customThe reaction was quenched by the careful addition of water
- concentrationthen concentrated in vacuo
- additionThe resultant residue was treated with water (1 L)
- customthe precipitate formed
- filtrationcollected by filtration
- customdried in vacuo at 35° C.
出典と根拠
- ORDレコード
- ord-90f47a48fca44a5c9d6519dfcaa71422
- 出典データセット
- uspto-grants-2014_07
- 特許番号
- US08785626B2
反応ノート
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