Carbon Dioxide → HCID 18548968、化合物

HRID 276825

反応式

HRID 276825 の反応式
C([Li])CCC.[CH3:6][O:7][CH2:8][CH2:9][N:10]([CH3:14])[CH2:11][C:12]#[CH:13].[C:15](=[O:17])=[O:16].O>CCCCCC.O1CCCC1.CO>[CH3:6][O:7][CH2:8][CH2:9][N:10]([CH3:14])[CH2:11][C:12]#[C:13][C:15]([OH:17])=[O:16]

参加物

8

反応物 4

HCID 280Carbon DioxideHCID 962WaterHCID 18548974(2-Methoxyethyl)(methyl)(prop-2-yn-1-yl)amineHCID 178418339Butyllithium

生成物 1

HCID 18548968HCID 18548968、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

n-Butyl lithium in hexane (37.8 mL, 2.5 M in n-hexane) was slowly added to (2-methoxy-ethyl)-methyl-prop-2-ynyl-amine (12.0 g, 94.5 mmol) in 90 mL of tetrahydrofuran under nitrogen. The mixture was stirred for 1 hr at −78° C., then dry carbon dioxide was passed through the reaction overnight. The resulting solution was poured into water and washed with ethyl acetate. The aqueous layer was evaporated under reduced pressure to give the crude acid. The dry acid was dissolved in methanol, and the insoluble salt was removed via filtration. The filtrate was collected and dried in vacuo to give 15 g of 4-[(2-methoxy-ethyl)-methyl-amino]-but-2-ynoic acid: mass spectrum (m/e): M−H 170.

後処理

  1. washwashed with ethyl acetate
  2. customThe aqueous layer was evaporated under reduced pressure
  3. customto give the crude acid
  4. customthe insoluble salt was removed via filtration
  5. customThe filtrate was collected
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-cd7a2059620a4983985f1047748d12a9
出典データセット
uspto-grants-2002_03
特許番号
US06355636B1

関連ノート

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