Acetone → 3-(1,1-Dimethylpropyl)-6,6-dimethylfulvene

HRID 495737노트

반응식

HRID 495737 반응식
[CH3:1][C:2]([C:6]1[CH2:10][CH:9]=[CH:8][CH:7]=1)([CH3:5])[CH2:3][CH3:4].[CH3:11][C:12]([CH3:14])=O.N1CCCC1>CO.CCOCC.O>[CH3:1][C:2]([C:6]1[CH:10]=[CH:9][C:8](=[C:12]([CH3:14])[CH3:11])[CH:7]=1)([CH3:5])[CH2:3][CH3:4]

참가 물질

7

반응물 3

HCID 180AcetoneHCID 31268PyrrolidineHCID 12779334(1,1-Dimethylpropyl)cyclopentadiene

생성물 1

HCID 178181473-(1,1-Dimethylpropyl)-6,6-dimethylfulvene수율 48%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 3.00 g (22.0 mmol) of (1,1-dimethylpropyl)cyclopentadiene in 30 ml of methanol, 16.2 ml (220.4 mmol) of acetone and 3.7 ml (44.0 mmol) of pyrrolidine were added with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 100 ml of ether, 50 ml of water was added. The organic phase was separated, washed with water and a saturated saline solution, then dried over anhydrous magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was subjected to vacuum distillation (100° C./1 mmHg) to obtain 1.85 g (10.49 mmol) of a yellow liquid (yield: 48%). The analyzed values are given below.

후처리

  1. additionwas added
  2. customThe organic phase was separated
  3. washwashed with water
  4. dry with materiala saturated saline solution, then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customFrom the filtrate, the solvent was removed under reduced pressure
  7. customto obtain a liquid
  8. distillationThe liquid was subjected to vacuum distillation (100° C./1 mmHg)

출처 및 근거

ORD 기록
ord-5eb6c241f9ea4659a6bddf20c5bbf8c6
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939928B1

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