Nitrogen → HCID 57960183、化合物

HRID 82843ノート

反応式

HRID 82843 の反応式
N#N.[OH:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[N:9]=1.[CH3:14]I>C(Cl)Cl>[CH3:14][O:3][CH2:4][C:5]1[O:6][CH:7]=[C:8]([C:10]([O:12][CH3:13])=[O:11])[N:9]=1

参加物

5

反応物 3

HCID 947NitrogenHCID 6328Methyl iodideHCID 67281821Methyl 2-(hydroxymethyl)oxazole-4-carboxylate

生成物 1

HCID 57960183HCID 57960183、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
40 °C

実験手順

In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of methyl 2-(hydroxymethyl)oxazole-4-carboxylate (231 mg, 1.47 mmol) in CH2Cl2 (0.9 mL) was treated with MeI (0.11 mL, 1.76 mmol) followed by Ag2O (511 mg, 2.21 mmol) and the resulting mixture (protected from light) was stirred overnight at 40° C. The reaction mixture was filtered and the solvent was removed under reduced pressure. Purification of the residue by FC (1:1 hept-EA) gave the title compound as a colorless oil: TLC: rf (1:1 hept-EA)=0.33. LC-MS-conditions 07: tR=0.49 min, [M+H]+=172.20.

後処理

  1. filtrationThe reaction mixture was filtered
  2. customthe solvent was removed under reduced pressure
  3. customPurification of the residue by FC (1:1 hept-EA)

出典と根拠

ORDレコード
ord-4bb216c17d44415d9ff82aa4f3b5dbd9
出典データセット
uspto-grants-2014_09
特許番号
US08846733B2

反応ノート

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