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

HRID 1093023노트

반응식

HRID 1093023 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e3c1ebf2080248a0b355853819c31190
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129541B2

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