Diisopropylethylamine → 1-Cyclohexyl-2-isocyanatobenzene

HRID 1097823ノート

反応式

HRID 1097823 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 574747361-Cyclohexyl-2-isocyanatobenzene

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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 diphenylphosphoryl 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.

後処理

  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

出典と根拠

ORDレコード
ord-f3fcec60ef7640e4b1e5822b980dbe1c
出典データセット
uspto-grants-2012_03
特許番号
US08143277B2

反応ノート

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