Lawesson's reagent → HCID 5324342、化合物

HRID 1099097

反応式

HRID 1099097 の反応式
COC1C=CC(P2(=S)SP(C3C=CC(OC)=CC=3)(=S)[S:10]2)=CC=1.[C:23]([O:27][C:28](=[O:35])[NH:29][C@H:30]([CH3:34])[C:31]([NH2:33])=O)([CH3:26])([CH3:25])[CH3:24]>COCCOC>[C:23]([O:27][C:28](=[O:35])[NH:29][C@H:30]([CH3:34])[C:31]([NH2:33])=[S:10])([CH3:26])([CH3:25])[CH3:24]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 7015296Boc-D-Ala-NH2

生成物 1

HCID 5324342HCID 5324342、化合物収率 203.5%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

2,4-Bis(4-methoxyphenyl)-2,4-dithioxo-1,3,2,4-dithiadiphosphetane (1.6 g, 0.0038 mol) was added to a solution of tert-butyl[(1R)-2-amino-1-methyl-2-oxoethyl]carbamate (1.45 g, 0.00770 mol) in 1,2-dimethoxyethane (40 mL). The resulting suspension was stirred at RT for 5 h. After removal of solvent the residue was taken up into ethyl acetate. It was washed with 0.1 N NaOH solution, water, brine; dried over Na2SO4. After filtration the filtrate was concentrated to yield 1.58 g of the product. (yield: ˜100%).

後処理

  1. customAfter removal of solvent the residue
  2. washIt was washed with 0.1 N NaOH solution, water, brine
  3. dry with materialdried over Na2SO4
  4. filtrationAfter filtration the filtrate
  5. concentrationwas concentrated

出典と根拠

ORDレコード
ord-2367931cdfd842fa98bc713e4691fa14
出典データセット
uspto-grants-2012_03
特許番号
US08143251B2

関連ノート

読み込み中…