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Chlorosuccinimide → HCID 86707797, 화합물

HRID 2174387
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HRID 2174387 반응식
[CH3:1][O:2][C:3]([CH:5]1[CH2:8][N:7]([C:9]2[CH:14]=[CH:13][C:12]([CH:15]=[N:16][OH:17])=[CH:11][CH:10]=2)[CH2:6]1)=[O:4].[Cl:18]N1C(=O)CCC1=O.C(=O)([O-])O.[K+].[Cl:31][C:32]1[CH:37]=[C:36]([C:38]([C:40]([F:43])([F:42])[F:41])=[CH2:39])[CH:35]=[C:34]([Cl:44])[C:33]=1[Cl:45]>CN(C=O)C>[CH3:1][O:2][C:3]([CH:5]1[CH2:8][N:7]([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH2:39][C:38]([C:36]4[CH:37]=[C:32]([Cl:31])[C:33]([Cl:45])=[C:34]([Cl:44])[CH:35]=4)([C:40]([F:42])([F:43])[F:41])[O:17][N:16]=3)=[CH:11][C:10]=2[Cl:18])[CH2:6]1)=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 31398ChlorosuccinimideHCID 516893Potassium BicarbonateHCID 498201551,2,3-Trichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzeneHCID 867077941-[4-(Hydroxyimino-methyl)-phenyl]-azetidine-3-carboxylic acid methyl ester

생성물 1

HCID 86707797HCID 86707797, 화합물수율 38.6%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
45 °C

실험 절차

To a stirred solution of 1-[4-(hydroxyimino-methyl)-phenyl]-azetidine-3-carboxylic acid methyl ester (Preparation 10, 0.95 g, 4.059 mmol, 1 eq.) in DMF (10 mL) was added N-chloro succinimide (0.59 g, 4.46 mmol) at room temperature. Resulting reaction mixture was stirred at 45° C. for 30 minutes. After complete consumption of starting material to chloro intermediate, reaction mixture was cooled to room temperature, potassium hydrogen carbonate (0.61 g, 6.089 mmol) was added followed by of 1,2,3-trichloro-5-(1-trifluoromethyl-vinyl)-benzene (1.33 g, 4.87 mmol) at room temperature. Resulting reaction mixture was stirred at room temperature for 18 hours under nitrogen atmosphere. After consumption of chloro intermediate, reaction mixture was quenched with ice cold water (250 mL) and extracted with EtOAc (2×200 mL). Combined organic layer was dried over anhydrous sodium sulphate and concentrated in vacuo to 1 g crude. Crude compound was purified by column chromatography (silica gel, 100-200 mesh) to afford 0.850 g impure product. Impure product was repurified by column chromatography (silica gel, 100-200 mesh) to afford 0.55 g. 1H NMR (400 MHz, CDCl3): 3.51-3.55 (m, 1H), 3.60 (d, 1H, J=17.08 Hz), 3.75 (s, 3H), 4.0 (d, 1H, J=17.04 Hz), 4.28 (t, 2H, J=7.2 Hz), 4.36 (t, 2H, J=8.36 Hz), 6.45 (d, 1H, J=8.6 Hz), 7.41 (dd, 1H, J1=1.92 Hz, J2=8.6 Hz), 7.46 (d, 1H, J=1.88 Hz), 7.62 (s, 2H); LC-MS (M+H): =542.50.

후처리

  1. customResulting
  2. customreaction mixture
  3. customAfter complete consumption of starting material
  4. customto chloro intermediate, reaction mixture
  5. temperaturewas cooled to room temperature
  6. customResulting
  7. customreaction mixture
  8. stirringwas stirred at room temperature for 18 hours under nitrogen atmosphere
  9. customAfter consumption of chloro intermediate, reaction mixture
  10. customwas quenched with ice cold water (250 mL)
  11. extractionextracted with EtOAc (2×200 mL)
  12. dry with materialCombined organic layer was dried over anhydrous sodium sulphate
  13. concentrationconcentrated in vacuo to 1 g crude
  14. customCrude compound was purified by column chromatography (silica gel, 100-200 mesh)

출처 및 근거

ORD 기록
ord-2fe2e59a7f0442299ff452272eac2992
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09061013B2

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