Sodium diethyldithiocarbamate trihydrate → 3-(Benzyloxycarbonylamino)-N-[2-[diethylamino(thiocarbonyl)-thio]ethyl]propionamide

HRID 1583509

反応式

HRID 1583509 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][C:14]([NH:16][CH2:17][CH2:18]Br)=[O:15])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.O.O.[CH2:23]([N:25]([CH2:29][CH3:30])[C:26](=[S:28])[S-:27])[CH3:24].[Na+]>CC(C)=O>[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][C:14]([NH:16][CH2:17][CH2:18][S:28][C:26]([N:25]([CH2:29][CH3:30])[CH2:23][CH3:24])=[S:27])=[O:15])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 517546Sodium diethyldithiocarbamate trihydrateHCID 202587523-(benzyloxycarbonylamino)-N-(2-bromoethyl)propionamide

生成物 1

HCID 133361483-(Benzyloxycarbonylamino)-N-[2-[diethylamino(thiocarbonyl)-thio]ethyl]propionamide収率 89.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

To the solution of 3-(benzyloxycarbonylamino)-N-(2-bromoethyl)propionamide (10 g) in acetone (250 ml), sodium diethyldithiocarbamate trihydrate (6.8 g) in acetone (150 ml) is added and the mixture is stirred for 40 minutes at room temperature. The reaction mixture is filterd and the filtrate is concentrated in vacuo. The residue is dissolved in ethyl acetate (150 ml) and the solution is washed with N hydrochloric acid, N sodium hydroxide, water and saturated sodium chloride solution in the named order. The ethyl acetate solution is dried over anhydrous magnesium sulfate and concentrated in vacuo to give 10.7 g (89%) of the titled compound.

後処理

  1. concentrationthe filtrate is concentrated in vacuo
  2. dissolutionThe residue is dissolved in ethyl acetate (150 ml)
  3. washthe solution is washed with N hydrochloric acid, N sodium hydroxide, water and saturated sodium chloride solution in the named order
  4. dry with materialThe ethyl acetate solution is dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d85aec25f98640f0976d1ec51fba414a
出典データセット
uspto-grants-1985_11
特許番号
US04552765

関連ノート

読み込み中…