Lawesson's reagent → 2-(Tert-butyldiphenylsilyloxy)propanethioamide

HRID 872858

反応式

HRID 872858 の反応式
COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:10]2)=CC=1.[Si:23]([O:40][CH:41]([CH3:45])[C:42]([NH2:44])=O)([C:36]([CH3:39])([CH3:38])[CH3:37])([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C1COCC1>[Si:23]([O:40][CH:41]([CH3:45])[C:42](=[S:10])[NH2:44])([C:36]([CH3:39])([CH3:38])[CH3:37])([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 671685282-(Tertbutyldiphenylsilyloxy)propanamide

生成物 1

HCID 872949642-(Tert-butyldiphenylsilyloxy)propanethioamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

A flask containing 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (387 mg, 0.957 mmol) was put under nitrogen atmosphere. 2-(tert-butyldiphenylsilyloxy)propanamide (622 mg, 1.899 mmol) dissolved in dry THF (10 ml) was added, temperature was raised to 60° C. and the mixture was allowed to react for 3 h. The solvent was evaporated and the product was extracted from DCM/water. The product was used in the next step without further purification. LC-MS: [M+1]=344.56.

後処理

  1. additionwas added
  2. customto react for 3 h
  3. customThe solvent was evaporated
  4. extractionthe product was extracted from DCM/water
  5. customThe product was used in the next step without further purification

出典と根拠

ORDレコード
ord-55ce6e08d68e4ee2846797447671d860
出典データセット
uspto-grants-2015_03
特許番号
US08975254B2

関連ノート

読み込み中…