Formic Acid → 4-Formylmorpholine-3-carboxylic acid

HRID 926347ノート

反応式

HRID 926347 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8].[CH:10](O)=[O:11].C(OC(=O)C)(=O)C>O>[CH:10]([N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8])=[O:11]

参加物

5

反応物 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 33401523-Morpholinecarboxylic acid

生成物 1

HCID 655465344-Formylmorpholine-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
2.5 °C

実験手順

To a mixture of morpholine-3-carboxylic acid (5 g, 38.1 mmol) and formic acid (46.6 g, 1.01 mol) cooled at 0-5° C. was added acetic anhydride (26.7 g, 262 mmol) dropwise. The resulting mixture was stirred at room temperature for 2 h. An excess of water was added while cooling the mixture. The resulting mixture was then concentrated under reduced pressure. The crude product 4-formyl-morpholine-3-carboxylic acid (6 g) was used in the next step without further purification. LC/MS (method 7): Rt=0.13 min; m/z=160.1 (M+H+).

後処理

  1. temperaturewhile cooling the mixture
  2. concentrationThe resulting mixture was then concentrated under reduced pressure
  3. customThe crude product 4-formyl-morpholine-3-carboxylic acid (6 g) was used in the next step without further purification

出典と根拠

ORDレコード
ord-0be6712826f34056b9e1d39b23a97a1f
出典データセット
uspto-grants-2016_03
特許番号
US09284333B2

反応ノート

読み込み中…