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

HRID 1093023ノート

反応式

HRID 1093023 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, 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. washwashed through with DCM (500 ml)
  5. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-e3c1ebf2080248a0b355853819c31190
出典データセット
uspto-grants-2012_03
特許番号
US08129541B2

反応ノート

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