碘甲烷 → 2-氧代-1-甲基-烟酸

HRID 1908115笔记

反应方程式

HRID 1908115 反应方程式
[O:1]=[C:2]1[C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=[CH:4][NH:3]1.[OH-].[K+].I[CH3:14]>CO.O>[CH3:14][N:3]1[CH:4]=[CH:5][CH:6]=[C:7]([C:8]([OH:10])=[O:9])[C:2]1=[O:1]

参与物

6

反应物 3

HCID 6328碘甲烷HCID 14797氢氧化钾HCID 691142-羟基烟酸

产物 1

HCID 12015102-氧代-1-甲基-烟酸

试剂、催化剂与溶剂 2

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

To 2-oxo-1H-pyridine-3-carboxylic acid (2.00 g, 14.4 mmol) in methanol (20 mL) was added a solution of KOH (1.60 g, 28.5 mmol) in water (3 mL) and the mixture was vigorously stirred until a thick suspension formed. Iodomethane (10 μL, 0.16 mmol) was added and the mixture was heated at reflux for 1.5 h. The mixture was concentrated to ⅓ volume and was acidified to pH 1 with 6N HCl. The solids were filtered off and were washed with water (3×2 mL) and acetonitrile (2×2 mL), and then dried in vacuo to give 1-methyl-2-oxo-pyridine-3-carboxylic acid as a white solid. ESI-MS m/z calc 153.0. found 154.1 (M−1)−. Retention time: 0.65 minutes (3 min run).

后处理

  1. customformed
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 1.5 h
  4. concentrationThe mixture was concentrated
  5. filtrationThe solids were filtered off
  6. washwere washed with water (3×2 mL) and acetonitrile (2×2 mL)
  7. customdried in vacuo

来源与证据

ORD记录
ord-03398f8c8f004d69ba67d611336215a2
来源数据集
uspto-grants-2013_12
专利号
US08598164B2

反应笔记

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