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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
ノート
印刷プレビュー

反応式

HRID 1854588 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 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
収率 89.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-034535f778ac4272ba483033ef74c1d8
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962654B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート