Water → HCID 14993186、化合物

HRID 486716ノート

反応式

HRID 486716 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 14993186HCID 14993186、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6c4ea074ef4c4228a86f46b603155c44
出典データセット
uspto-grants-1994_03
特許番号
US05292767

反応ノート

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