Hydrochloric Acid → 2-Benzyloxycarbonylamino-3-(2,4-dichlorobenzenesulfonylamino)-2-methylpropionic Acid

HRID 1994434노트

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HRID 1994434 반응식
[CH2:1]([O:8][C:9]([NH:11][C:12]([CH3:30])([CH2:17][NH:18][S:19]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[Cl:29])(=[O:21])=[O:20])[C:13]([O:15]C)=[O:14])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].C([O-])(O)=O.[Na+].Cl>CO.O>[CH2:1]([O:8][C:9]([NH:11][C:12]([CH3:30])([CH2:17][NH:18][S:19]([C:22]1[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][C:23]=1[Cl:29])(=[O:20])=[O:21])[C:13]([OH:15])=[O:14])=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 68695213Methyl 2-benzyloxycarbonylamino-3-(2,4-dichlorobenzenesulfonylamino)-2-methylpropionate

생성물 1

HCID 686938982-Benzyloxycarbonylamino-3-(2,4-dichlorobenzenesulfonylamino)-2-methylpropionic Acid수율 87.7%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매2회

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온도
60 °C

실험 절차

0.08 g (0.168 mmol) of methyl 2-benzyloxycarbonylamino-3-(2,4-dichlorobenzenesulfonylamino)-2-methylpropionate and 0.093 g (0.674 mmol) of potassium carbonate are stirred in a mixture of 4.5 ml of MeOH and 0.5 ml of water for 90 min. Then 3 ml of saturated NaHCO3 solution are added, and the mixture is stirred at 60° C. for 2 h. 0.5 ml of water is added, followed by 4N HCl (aq) until a pH of 2 is reached. The solution is extracted 3 times with 10 ml of EtOAc each time, the combined organic phases are dried over MgSO4, and the solvent is removed in vacuo. 68 mg of the desired product are obtained. MW=460 (calculated, monoisotopic), measured value: (M+H)+461.

후처리

  1. extractionThe solution is extracted 3 times with 10 ml of EtOAc each time
  2. dry with materialthe combined organic phases are dried over MgSO4
  3. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-5b6693dda13d4be4b94dd3017b70533b
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652007B2

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