Iodine → Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

HRID 601620ノート

反応式

HRID 601620 の反応式
II.C(N(CC)CC)C.[CH2:10]([O:17][C:18](=[O:30])[NH:19][CH2:20][CH2:21][C:22](=[O:29])[NH:23][CH2:24][C:25](=O)[CH2:26][CH3:27])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(Cl)Cl>[CH2:10]([O:17][C:18](=[O:30])[NH:19][CH2:20][CH2:21][C:22]1[O:29][C:25]([CH2:26][CH3:27])=[CH:24][N:23]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 807IodineHCID 8471TriethylamineHCID 57637089Benzyl [2-(2-oxobutylcarbamoyl)ethyl]carbamate

生成物 1

HCID 57636953Benzyl [2-(5-ethyloxazol-2-yl)ethyl]carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred suspension of polymer supported triphenylphosphene (19.6 g, 58.9 mmol) in DCM (250 ml) is added iodine (14.95 g, 58.9 mmol). After stirring at room temperature for 10 minutes, the mixture is treated with triethylamine (16.4 ml, 117.5 mmol) followed by a solution of [2-(2-oxo-butylcarbamoyl)-ethyl]-carbamic acid benzyl ester (step 2) (6.88 g, 23.5 mmol) in DCM (50 ml). The reaction mixture is stirred overnight and then filtered through Celite™ filter material, washed through with DCM (500 ml) and the solvent removed in vacuo to yield the titled compound as a brown solid.

後処理

  1. additionTo a stirred suspension of polymer
  2. stirringThe reaction mixture is stirred overnight
  3. filtrationfiltered through Celite™
  4. filtrationfilter material
  5. washwashed through with DCM (500 ml)
  6. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-67442e85c73b407b8d9d4c3bba5f9a25
出典データセット
uspto-grants-2011_03
特許番号
US07902375B2

反応ノート

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