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Triethylamine → methyl (1S,3R)-3-[[tert-butyl(dimethyl)silyl]oxymethyl]-2-[2-(6-chloro-2-fluoro-3-methoxy-phenyl)acetyl]-1-methyl-3,4-dihydro-1H-isoquinoline-5-carboxylate

HRID 1854588
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HRID 1854588 반응식
C(N(CC)CC)C.[Si:8]([O:15][CH2:16][C@H:17]1[CH2:26][C:25]2[C:24]([C:27]([O:29][CH3:30])=[O:28])=[CH:23][CH:22]=[CH:21][C:20]=2[C@H:19]([CH3:31])[NH:18]1)([C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:10])[CH3:9].F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1.[Cl:65][C:66]1[C:71]([CH2:72][C:73](O)=[O:74])=[C:70]([F:76])[C:69]([O:77][CH3:78])=[CH:68][CH:67]=1.[Cl-].[NH4+]>CN(C)C=O>[Si:8]([O:15][CH2:16][C@H:17]1[CH2:26][C:25]2[C:24]([C:27]([O:29][CH3:30])=[O:28])=[CH:23][CH:22]=[CH:21][C:20]=2[C@H:19]([CH3:31])[N:18]1[C:73](=[O:74])[CH2:72][C:71]1[C:66]([Cl:65])=[CH:67][CH:68]=[C:69]([O:77][CH3:78])[C:70]=1[F:76])([C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:9])[CH3:10]
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참가 물질

7

반응물 5

HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 2724699PyBOPHCID 467375092-(6-Chloro-2-fluoro-3-methoxyphenyl)acetic acidHCID 123884369methyl (1S,3R)-3-[[tert-butyl(dimethyl)silyl]oxymethyl]-1-methyl-1,2,3,4-tetrahydroisoquinoline-5-carboxylate

생성물 1

HCID 123499849
methyl (1S,3R)-3-[[tert-butyl(dimethyl)silyl]oxymethyl]-2-[2-(6-chloro-2-fluoro-3-methoxy-phenyl)acetyl]-1-methyl-3,4-dihydro-1H-isoquinoline-5-carboxylate
수율 89.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Add triethylamine (0.36 mL, 2.57 mmol) to a stirred solution of methyl (1S,3R)-3-[[tert-butyl(dimethyl)silyl]oxymethyl]-1-methyl-1,2,3,4-tetrahydroisoquinoline-5-carboxylate (500 mg, 1.29 mmol), (benzotriazol-1-yloxy)tripyrrolidinophosphonium hexafluorophosphate (1.02 g, 1.93 mmol) and 2-(6-chloro-2-fluoro-3-methoxy-phenyl)acetic acid (356 mg, 1.54 mmol) in dimethylformamide (6.4 mL). Stir at room temperature for 16 h. Add saturated aqueous ammonium chloride (60 mL). Extract with ethyl acetate (3×50 mL). Wash the combined organic layers with brine. Dry over magnesium sulfate, filter and concentrate under reduced pressure. Purify by flash chromatography to yield the title compound as an amorphous yellow solid (703 mg, 1.15 mmol): MS (m/z): 550.0 (M+1).

후처리

  1. extractionExtract with ethyl acetate (3×50 mL)
  2. washWash the combined organic layers with brine
  3. dry with materialDry over magnesium sulfate
  4. filtrationfilter
  5. concentrationconcentrate under reduced pressure
  6. customPurify by flash chromatography

출처 및 근거

ORD 기록
ord-034535f778ac4272ba483033ef74c1d8
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08962654B2

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