Water → tert-Butyl [2-(5-oxo-4,5-dihydro[1,3,4]oxadiazol-2-yl)thiophen-3-yl]carbamate

HRID 460314ノート

反応式

HRID 460314 の反応式
[C:1](Cl)(Cl)=[O:2].[C:5]([O:9][C:10]([NH:12][C:13]1[CH:17]=[CH:16][S:15][C:14]=1[C:18]([NH:20][NH2:21])=[O:19])=[O:11])([CH3:8])([CH3:7])[CH3:6].O>C1COCC1>[O:2]=[C:1]1[O:19][C:18]([C:14]2[S:15][CH:16]=[CH:17][C:13]=2[NH:12][C:10](=[O:11])[O:9][C:5]([CH3:8])([CH3:6])[CH3:7])=[N:20][NH:21]1

参加物

5

反応物 3

HCID 962WaterHCID 6371PhosgeneHCID 184459443-(tert-Butoxycarbonylamino)thiophene-2-carboxylic hydrazide

生成物 1

HCID 86760474tert-Butyl [2-(5-oxo-4,5-dihydro[1,3,4]oxadiazol-2-yl)thiophen-3-yl]carbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4 ml of a 20% toluenic phosgene solution are added dropwise to a solution of 240 mg of 3-(tert-butoxycarbonylamino)thiophene-2-carboxylic hydrazide in 5 ml of THF and the mixture is stirred at RT. After one hour, the mixture is admixed with 10 ml of water and, after brief digestion, extracted with ethyl acetate. After the ethyl acetate phase has been dried over sodium sulfate, the mixture is concentrated under reduced pressure and the remaining residue is used further without further purification.

後処理

  1. extractionafter brief digestion, extracted with ethyl acetate
  2. dry with materialAfter the ethyl acetate phase has been dried over sodium sulfate
  3. concentrationthe mixture is concentrated under reduced pressure
  4. customthe remaining residue is used further without further purification

出典と根拠

ORDレコード
ord-37189ac45f724e52911353c37347c860
出典データセット
uspto-grants-2007_03
特許番号
US07196114B2

反応ノート

読み込み中…