Methyl Acetate → HCID 68864196, 화합물

HRID 229109

반응식

HRID 229109 반응식
[C:1]1([CH:7]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:8][NH:9][CH2:10][CH2:11][C@@H:12]([CH3:24])[O:13][C:14]2[CH:15]=[C:16]([CH2:20][C:21]([OH:23])=[O:22])[CH:17]=[CH:18][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:31][C:32]([F:43])([F:42])[C:33]1[CH:34]=[C:35]([CH:38]=[CH:39][C:40]=1[F:41])[CH:36]=O.COC(=O)C.[Cl:49]C1C(C(F)(F)F)=CC=CC=1C=O.Cl.CCOCC>CCOCC>[ClH:49].[F:42][C:32]([F:31])([F:43])[C:33]1[CH:34]=[C:35]([CH:38]=[CH:39][C:40]=1[F:41])[CH2:36][N:9]([CH2:8][CH:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)[CH2:10][CH2:11][C@@H:12]([CH3:24])[O:13][C:14]1[CH:15]=[C:16]([CH2:20][C:21]([OH:23])=[O:22])[CH:17]=[CH:18][CH:19]=1

참가 물질

7

반응물 5

HCID 6584Methyl AcetateHCID 5222694-Fluoro-3-(trifluoromethyl)benzaldehydeHCID 27366722-Chloro-3-(trifluoromethyl)benzaldehydeHCID 10953452Ether hydrochlorideHCID 68864815(R)-2-(3-{3-[(2,2-diphenylethyl)amino]-1-methyl-propoxy}phenyl)acetic acid

생성물 1

HCID 68864196HCID 68864196, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Following the procedure of Example 7(d) except (R)-2-(3-{3-[(2,2-diphenylethyl)amino]-1-methyl-propoxy}-phenyl)acetic acid and 3-(trifluoromethyl)-4-fluoro-benzaldehyde were used instead of (R)-2-(3-{3-(2,2-diphenylethyl)amino]-3-methyl-propoxy}phenyl)acetic acid methyl ester and 2-chloro-3-trifluoromethylbenzaldehyde in step (d) the corresponding carboxylic acid was obtained. The crude product was purified by preparative HPLC (TMC CombiPrep PDS, 75×30 mm, 25 mL/min, acetonitrile: H2O, UV detection at 254 nm) to afford the free base. The resulting amine/carboxylic acid was dissolved in Et2O (diethylether) and acidified with 1.0 M HCl/Et2O. The reaction mixture was concentrated in vacuo and dried under reduced pressure to give the title compound as a white solid, 95 mg (88%). MS (ESI) 580.6 (M+H+).

후처리

  1. customwas obtained
  2. customThe crude product was purified by preparative HPLC (TMC CombiPrep PDS, 75×30 mm, 25 mL/min, acetonitrile: H2O, UV detection at 254 nm)
  3. customto afford the free base
  4. concentrationThe reaction mixture was concentrated in vacuo
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-04f1056c8c994635b795ee80ded4a5ce
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560586B2

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