Diisopropylethylamine → 1-Cyclohexyl-2-isocyanatobenzene

HRID 2099492노트

반응식

HRID 2099492 반응식
[CH:1]1([C:7]2[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=2C(O)=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CC[N:18]([CH:22](C)C)C(C)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:32])C=CC=CC=1>C1(C)C=CC=CC=1>[CH:1]1([C:7]2[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=2[N:18]=[C:22]=[O:32])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 70205722-cyclohexylbenzoic Acid

생성물 1

HCID 574747361-Cyclohexyl-2-isocyanatobenzene

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a stirred solution of 2-cyclohexylbenzoic acid (2 g, 9.8 mmol) and DIPEA (3.45 μL, 14.7 mmol) in toluene (25 mL) under nitrogen was added diphenylphosphoroyl azide (2.1 mL, 9.8 mmol). The reaction mixture was stirred for 4 h at room temperature and then heated at 90° C. for 3 h. Upon cooling, the organic layer was washed with saturated ammonium chloride solution (2×10 mL) and brine (1×10 mL), dried (MgSO4), filtered and the solvent removed under reduced pressure to give the title compound as a clear amber oil.

후처리

  1. temperatureheated at 90° C. for 3 h
  2. temperatureUpon cooling
  3. washthe organic layer was washed with saturated ammonium chloride solution (2×10 mL) and brine (1×10 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-3dee879f8092454daa23c9ae6829ed0a
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07569586B2

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