4-Chloro-2-methylphenyl isocyanate → HCID 57527884, 화합물

HRID 339417

반응식

HRID 339417 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][NH:2]1.[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([N:17]=[C:18]=[O:19])=[C:13]([CH3:20])[CH:12]=1>O1CCOCC1>[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18]([N:2]2[CH2:3][C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[CH2:1]2)=[O:19])=[C:13]([CH3:20])[CH:12]=1

참가 물질

4

반응물 2

HCID 1421574-Chloro-2-methylphenyl isocyanateHCID 422478Isoindoline

생성물 1

HCID 57527884HCID 57527884, 화합물수율 94.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of isoindoline (238 mg, 2.0 mmol) in dry 1,4-dioxane (10 mL) was added 4-chloro-2-methylphenyl isocyanate (335 mg, 2.0 mmol) under argon at room temperature. The reaction mixture was then stirred at RT overnight. The solvent was evaporated under reduced pressure, and the residue was purified by recrystallization from ethanol to give the title compound (540 mg, 94%) as a white solid. 1H NMR (500 MHz, DMSO-d6): δ 2.24 (s, 2H), 4.76 (s, 4H), 7.20 (dd, J=2.5, 8.5 Hz, 1H), 7.27 (d, J=2.5 Hz, 1H), 7.30-7.32 (m, 2H), 7.34-7.37 (m, 2H), 7.42 (d, J=8.5 Hz, 1H), 7.84 (s, 1H); 13C NMR (DMSO-d6): δ 17.7, 51.9, 122.8, 125.6, 126.8, 127.3, 128.1, 129.5, 134.7, 136.8, 154.2; MS (MH+, 287); EA calc'd for C16H15ClN2O: C, 67.02; H, 5.27; N, 9.77. Found C, 66.82; H, 5.41; N, 9.92.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by recrystallization from ethanol

출처 및 근거

ORD 기록
ord-8420e8bdee424cdc94fc4c766b82b133
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895050B2

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