Triethylamine → HCID 53719220、化合物

HRID 1005519

反応式

HRID 1005519 の反応式
[OH:1][CH2:2][C:3]1[N:4]([CH2:20][CH3:21])[C:5]([S:11][C:12]2[CH:17]=[C:16]([Cl:18])[CH:15]=[C:14]([Cl:19])[CH:13]=2)=[C:6]([CH:8]([CH3:10])[CH3:9])[N:7]=1.[NH+]1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(O[C:44]1([O:50][CH2:51][CH2:52][CH2:53][CH3:54])[CH2:49][CH2:48][CH2:47][CH2:46]C1)CCC.C(N(CC)CC)C>C(Cl)Cl>[CH2:51]([O:50][C:44]1([O:1][CH2:2][C:3]2[N:4]([CH2:20][CH3:21])[C:5]([S:11][C:12]3[CH:17]=[C:16]([Cl:18])[CH:15]=[C:14]([Cl:19])[CH:13]=3)=[C:6]([CH:8]([CH3:9])[CH3:10])[N:7]=2)[CH2:46][CH2:47][CH2:48][CH2:49]1)[CH2:52][CH2:53][CH3:54]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2437181,1-DibutoxycyclohexaneHCID 473933(5-(3,5-Dichlorophenylthio)-1-ethyl-4-isopropyl-1H-imidazol-2-yl)methanolHCID 22033616Pyridinium.p-toluenesulfonate

生成物 1

HCID 53719220HCID 53719220、化合物収率 34%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-hydroxymethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-ethyl-1H-imidazole (19) (345 mg, 1 mmol) prepared in accordance with the method as described in WO 96/10019 (EXAMPLE 25) and p-toluenesulfonic acid pyridinium (264 mg, 1.05 mmol) in methylene chloride (5 ml) was added 1,1-dibutoxycyclohexane (2.14 g, 10.0 mmol), and stirred at room temperature for 20 hours. A drop of triethylamine was added to the reaction mixture , and the mixture was filtered to remove the precipitated insoluble matter. The filtrate was concentrated under reduced pressure. Hexane was added to the residue, and the mixture was filtered to remove the insoluble matter. The filtrate was purified by chromatography on an alumina column (eluate: toluene) to give the compound 20 (165 mg, 34%). Rf 0.41 (Al2O3 60, Type E, toluene).

後処理

  1. filtrationthe mixture was filtered
  2. customto remove the precipitated insoluble matter
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. additionHexane was added to the residue
  5. filtrationthe mixture was filtered
  6. customto remove the insoluble matter
  7. customThe filtrate was purified by chromatography on an alumina column (eluate: toluene)

出典と根拠

ORDレコード
ord-5b3f7ad41dbf4aa48d176520476b5aad
出典データセット
uspto-grants-2000_04
特許番号
US06054591

関連ノート

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