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Chlorosulfonic acid → HCID 86601723, 화합물

HRID 1784416
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HRID 1784416 반응식
[Cl:1][S:2]([OH:5])(=O)=[O:3].[CH2:6]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][CH:18]=1)[CH2:15][N:14]([C:19](=[O:24])[C:20]([F:23])([F:22])[F:21])[CH2:13][CH2:12]2)[CH3:7]>ClCCl>[CH2:6]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][C:18]=1[S:2]([Cl:1])(=[O:5])=[O:3])[CH2:15][N:14]([C:19](=[O:24])[C:20]([F:21])([F:22])[F:23])[CH2:13][CH2:12]2)[CH3:7]
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참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 86601722HCID 86601722, 화합물

생성물 1

HCID 86601723HCID 86601723, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of chlorosulfonic acid (0.48 mL) in dichloromethane (5 mL) at 0° C. was added dropwise a solution of 1-(6-ethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-2,2,2-trifluoro-ethanone (0.39 g, 1.43 mmol). The mixture was stirred at room temperature overnight before partitioning between water and dichloromethane. The organic layer was removed, dried over sodium sulfate, filtered and evaporated to dryness yielding the subtitled compound as a clear oil (0.34 g). 1H NMR δ (CDCl3) 1.46-1.63 (3H, t), 2.95-3.06 (2H, m), 3.80-3.95 (2H, m), 4.18-4.32 (2H, m), 4.69-4.80 (2H, d), 6.84-6.93 (1H, d), 7.70-7.79 (1H, d).

후처리

  1. custombefore partitioning between water and dichloromethane
  2. customThe organic layer was removed
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-92285f3590cb4cb1a48b6f87416fb2dd
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504392B2

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