Dichloromethane → HCID 86595065, 화합물

HRID 987277노트

반응식

HRID 987277 반응식
FC(F)(F)C(O)=O.C([O:10][C:11](=[O:40])[C@@H:12]([O:37][CH2:38][CH3:39])[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([NH:29]C(OC(C)(C)C)=O)=[CH:25][CH:24]=2)=[CH:16][CH:15]=1)C.[Cl:41]CCl>>[ClH:41].[NH2:29][C:26]1[CH:25]=[CH:24][C:23]([CH2:22][CH2:21][O:20][C:17]2[CH:18]=[CH:19][C:14]([CH2:13][C@H:12]([O:37][CH2:38][CH3:39])[C:11]([OH:40])=[O:10])=[CH:15][CH:16]=2)=[CH:28][CH:27]=1

참가 물질

4

반응물 3

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 118125123-{4-[2-(4-tert-butoxycarbonylaminophenyl)ethoxy]phenyl}-(S)-2-ethoxypropanoic acid ethyl ester

생성물 1

HCID 86595065HCID 86595065, 화합물수율 96.5%

실험 절차

Trifluoroacetic acid (12 ml; 0.0706 mole) was added to a solution of 3-{4-[2-(4-tert-butoxycarbonylaminophenyl)ethoxy]phenyl}-(S)-2-ethoxypropanoic acid ethyl ester (30 g; 0.065 mole) in dichloromethane (150 ml). The reaction mixture was stirred over night at room temperature and then washed three times with water. The organic phase was dried with magnesium sulfate and evaporated. 1H-NMR of the product showed a mixture of product and starting material. The crude product (27.3 g) was redissolved in ethyl acetate, ethyl acetate saturated with hydrochloric acid (500 ml) was added and the mixture was stirred over night at room temperature. Evaporation gave 24.7 g (96.5% yield) of 3-{4-[2-(4-aminophenyl)ethoxy]phenyl}-(S)-2-ethoxypropanoic acid hydro chloride.

후처리

  1. washwashed three times with water
  2. dry with materialThe organic phase was dried with magnesium sulfate
  3. customevaporated
  4. additiona mixture of product
  5. dissolutionThe crude product (27.3 g) was redissolved in ethyl acetate
  6. additionethyl acetate saturated with hydrochloric acid (500 ml) was added
  7. stirringthe mixture was stirred over night at room temperature
  8. customEvaporation

출처 및 근거

ORD 기록
ord-0afa3de3ded24d77b7b724fc7f0e29dc
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630600B1

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