Carbon Dioxide → HCID 18548968, 화합물

HRID 379154

반응식

HRID 379154 반응식
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]

참가 물질

8

반응물 4

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

생성물 1

HCID 18548968HCID 18548968, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

반응 조건

온도
-78 °C

실험 절차

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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-0b20c2c2df2f465cb0f450da62d2fda2
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297258B1

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