Acetone → Benzoyl Diacetamide Thiourea

HRID 2204452ノート

反応式

HRID 2204452 の反応式
[C:1]([N:9]=[C:10]=[S:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:12][C:13]([NH:15][C:16]([CH3:18])=[O:17])=[O:14].CC(C)=O>ClCCl>[NH2:9][C:10]([NH2:15])=[S:11].[CH3:12][C:13]([N:15]([C:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:16]([CH3:18])=[O:17])=[O:14]

参加物

5

反応物 3

HCID 180AcetoneHCID 12263DiacetamideHCID 68284Benzoyl isothiocyanate

生成物 1

HCID 86706832Benzoyl Diacetamide Thiourea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer, thermo-probe, nitrogen purge and pressure-equilibrated addition funnel was added benzoyl isothiocyanate (25.0 g, 0.150 mol) followed by dichloromethane (100 mL). The mixture was cooled in an ice-water bath at a temperature below 5° C., at which point diacetamide (15.3 g, 0.150 mol) and acetone as the solvent and dichloromethane (100 mL) were added slowly over a period of time of about 30 minutes. The ice-water bath was removed and the reaction mixture was stirred under a nitrogen purge overnight. The reaction mixture was then concentrated in vacuo at a temperature of 40° C. and then dried to constant weight in vacuo at a temperature of 50° C. and a pressure of <1 mTorr.

後処理

  1. customTo a 250 mL 3-neck RBF equipped with a condenser, magnetic stirrer
  2. customthermo-probe, nitrogen purge
  3. additionwere added slowly over a period of time of about 30 minutes
  4. customThe ice-water bath was removed
  5. custompurge overnight
  6. concentrationThe reaction mixture was then concentrated in vacuo at a temperature of 40° C.
  7. customdried to constant weight in vacuo at a temperature of 50° C.

出典と根拠

ORDレコード
ord-0f7125632dbf46dba7330f73b4ee4948
出典データセット
uspto-grants-2016_06
特許番号
US09365750B2

反応ノート

読み込み中…