Water → HCID 14993186, 화합물

HRID 486716노트

반응식

HRID 486716 반응식
Br[CH:2]([CH2:8][CH2:9][CH:10](Br)[C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:3]([O:5][CH2:6][CH3:7])=[O:4].O.O.O.O.O.O.O.O.O.[Na+].[Na+].[SH-:28].C(OCC)C.O>CN(C)C=O>[CH2:6]([O:5][C:3]([CH:2]1[CH2:8][CH2:9][CH:10]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[S:28]1)=[O:4])[CH3:7]

참가 물질

6

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 241588Diethyl 2,5-dibromohexanedioateHCID 16211516Sodium sulfide nonahydrate

생성물 1

HCID 14993186HCID 14993186, 화합물수율 72.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of diethyl 2,5-dibromoadipate (4.5 g) in dimethylformamide (15 ml), sodium sulfide enneahydrate (3.9 g) was added under nitrogen atmosphere and the mixture was stirred for 5 hours under ice-cooling. To the reaction mixture, diethyl ether and water were added. The organic layer was washed with saturated sodium chloride solution, dried over anhydrous magnesium sulfate and concentrated in vacuo. The oily residue was purified by a silica gel column chromatography to give 2.1 g (72%) of 2,5-diethoxycarbonyltetrahydrothiophene.

후처리

  1. temperaturecooling
  2. washThe organic layer was washed with saturated sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe oily residue was purified by a silica gel column chromatography

출처 및 근거

ORD 기록
ord-6c4ea074ef4c4228a86f46b603155c44
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292767

반응 노트

불러오는 중…