Water → (1,1-Dimethylpropyl)cyclopentadiene

HRID 270995노트

반응식

HRID 270995 반응식
[CH3:1][C:2]([CH2:8][CH3:9])=[C:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH3:10][Li].O>CCOCC>[CH3:1][C:2]([C:3]1[CH2:7][CH:6]=[CH:5][CH:4]=1)([CH3:10])[CH2:8][CH3:9]

참가 물질

5

반응물 3

HCID 962WaterHCID 5707046-Methyl-6-ethylfulveneHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 12779334(1,1-Dimethylpropyl)cyclopentadiene수율 93%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a solution of 8.00 g (66.6 mmol) of 6-methyl-6-ethylfulvene in 40 ml of ether, 66.0 ml (75.2 mmol) of an ether solution of methyllithium was dropwise added in an nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. Then, 30 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over 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 (165° C./270 mmHg) to obtain 8.40 g (61.66 mmol) of a light yellow liquid (yield: 93%) The analyzed values are given below.

후처리

  1. washThe separated organic phase was washed with water
  2. dry with materiala saturated saline solution, then dried over magnesium sulfate
  3. filtrationfiltered
  4. customFrom the filtrate, the solvent was removed under reduced pressure
  5. customto obtain a liquid
  6. distillationThe liquid was subjected to vacuum distillation (165° C./270 mmHg)

출처 및 근거

ORD 기록
ord-2aaf108bc2dd4e90ad3f20e1d6b73431
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449533B2

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