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Hydrochloric Acid → 4-[3-(3-Bromophenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoic acid

HRID 967634
ノート
印刷プレビュー

反応式

HRID 967634 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl.[O:10]=[C:11](Cl)OC(Cl)(Cl)Cl.[CH:18]1([C:24]2[CH:29]=[CH:28][C:27]([NH:30][CH2:31][C:32]3[CH:40]=[CH:39][C:35]([C:36]([OH:38])=[O:37])=[CH:34][CH:33]=3)=[CH:26][CH:25]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1>C(OCC)C.C(OCC)(=O)C.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]([NH:5][C:11](=[O:10])[N:30]([CH2:31][C:32]2[CH:40]=[CH:39][C:35]([C:36]([OH:38])=[O:37])=[CH:34][CH:33]=2)[C:27]2[CH:28]=[CH:29][C:24]([CH:18]3[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)=[CH:25][CH:26]=2)[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 10426DiphosgeneHCID 115623-BromoanilineHCID 223111294-[(4-Cyclohexylphenylamino)methyl]benzoic acid

生成物 1

HCID 223110904-[3-(3-Bromophenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoic acid収率 94%

試薬・触媒・溶媒 3

HCID 1140
Toluene
溶媒
HCID 3283Diethyl Ether溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

3-Bromoaniline (1.4 g, 8.1 mmol) was dissolved in diethyl ether (50 mL) and 3.5 M dry HCl in ethyl acetate (2.3 mL) was added. The mixture was concentrated in vacuo. The residue was added toluene (100 mL) and concentrated in vacuo. The residue was added toluene (100 mL) and diphosgene (8.1 g, 41 mmol) and the resulting mixture was refluxed for 1.5 hour. After cooling, the mixture was concentrated in vacuo. The residue was dissolved in toluene (100 mL) and concentrated in vacuo. The residue was dissolved in DMF (30 mL) and 4-[(4-cyclohexylphenylamino)methyl]benzoic acid (1.3 g, 4.1 mmol) was added. The mixture was stirred at room temperature for 16 hours. The mixture was added ethyl acetate (150 mL) and washed with water:brine (1:1) (2×100 mL). The organic phase was dried with sodium sulphate and concentrated in vacuo. The residue was purified by column chromatography on silica gel eluting first with a mixture of ethyl acetate:n-heptane:triethylamine (7:2:1), then with ethyl acetate and finally with methanol to afford 1.95 g (94%) of 4-[3-(3-bromophenyl)-1-(4-cyclohexylphenyl)ureidomethyl]benzoic acid.

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. additionThe residue was added toluene (100 mL)
  3. concentrationconcentrated in vacuo
  4. temperaturethe resulting mixture was refluxed for 1.5 hour
  5. temperatureAfter cooling
  6. concentrationthe mixture was concentrated in vacuo
  7. dissolutionThe residue was dissolved in toluene (100 mL)
  8. concentrationconcentrated in vacuo
  9. dissolutionThe residue was dissolved in DMF (30 mL)
  10. washwashed with water:brine (1:1) (2×100 mL)
  11. dry with materialThe organic phase was dried with sodium sulphate
  12. concentrationconcentrated in vacuo
  13. customThe residue was purified by column chromatography on silica gel eluting first with a mixture of ethyl acetate:n-heptane:triethylamine (7:2:1)

出典と根拠

ORDレコード
ord-f0b57381e7634d1585f3a5f8335b12bb
出典データセット
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06953812B2

反応ノート

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