5-(Pentan-2-ylidene)cyclopenta-1,3-diene → HCID 12779343, 화합물

HRID 271009노트

반응식

HRID 271009 반응식
[CH3:1][C:2]([CH2:8][CH2:9][CH3:10])=[C:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH3:11][Li]>C1COCC1.CCOCC.O>[CH3:1][C:2]([C:3]1[CH2:7][CH:6]=[CH:5][CH:4]=1)([CH3:11])[CH2:8][CH2:9][CH3:10]

참가 물질

6

반응물 2

HCID 129395315-(Pentan-2-ylidene)cyclopenta-1,3-dieneHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 12779343HCID 12779343, 화합물수율 82%

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 7.00 g (52.2 mmol) of 6-methyl-6-propylfulvene in 40 ml of THF, 50.3 ml (57.3 mmol) of an ether solution of methyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. After the reaction solution was diluted with 100 ml of ether, 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 (75° C./5-7 mmHg) to obtain 6.40 g (42.6 mmol) of a light yellow liquid (yield: 82%). The analyzed values are given below.

후처리

  1. additionwas added
  2. washThe separated organic phase was washed with water
  3. dry with materiala saturated saline solution, then dried over magnesium sulfate and filtered.° From the filtrate
  4. customthe solvent was removed under reduced pressure
  5. customto obtain a liquid
  6. distillationThe liquid was subjected to vacuum distillation (75° C./5-7 mmHg)

출처 및 근거

ORD 기록
ord-dc71ffc685f2477f81fa7fb60bda6cad
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449533B2

반응 노트

불러오는 중…