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Hydrochloric Acid → HCID 20060987、化合物

HRID 1085132
ノート
印刷プレビュー

反応式

HRID 1085132 の反応式
[Cl:1][C:2]1[N:6]([C:7]2[CH:18]=[CH:17][C:10]([C:11]([CH2:13][C:14]([O-:16])=O)=O)=[CH:9][CH:8]=2)[C:5]([CH3:19])=[N:4][C:3]=1[CH:20]1[O:24]CCO1.[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][C:29]([NH2:33])=[C:28]([NH2:34])[CH:27]=1.Cl>C1(C)C=CC=CC=1.C1COCC1>[CH3:25][C:26]1[C:31]([CH3:32])=[CH:30][C:29]2[NH:33][C:14](=[O:16])[CH2:13][C:11]([C:10]3[CH:9]=[CH:8][C:7]([N:6]4[C:2]([Cl:1])=[C:3]([CH:20]=[O:24])[N:4]=[C:5]4[CH3:19])=[CH:18][CH:17]=3)=[N:34][C:28]=2[CH:27]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 766354,5-Dimethyl-1,2-phenylenediamineHCID 20060984HCID 20060984、化合物

生成物 1

HCID 20060987HCID 20060987、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

A solution of 4-[5-chloro-4-(1,3-dioxolan-2-yl)-2-methylimidazol-1-yl]benzoylacetate from Preparation 5 (155 mg, 0.38 mmol), and 4,5-dimethyl-1,2-diaminobenzene (55 mg, 0.4 mmol) in toluene (4 ml) was heated at reflux for 4.5 hours, then evaporated to dryness and purified by flash chromatography (eluting with ethyl acetate) to afford a pale yellow gum. 1M HCl (2 ml) was added to a solution of the residue in THF (2 ml) and the mixture was heated to 70° C. for 1 hour. The THF was evaporated and the residue was partitioned between aqueous sodium bicarbonate and dichloromethane. The organic layer was dried over magnesium sulphate and evaporated.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 4.5 hours
  3. customevaporated to dryness
  4. custompurified by flash chromatography (eluting with ethyl acetate)
  5. customto afford a pale yellow gum
  6. customThe THF was evaporated
  7. customthe residue was partitioned between aqueous sodium bicarbonate and dichloromethane
  8. dry with materialThe organic layer was dried over magnesium sulphate
  9. customevaporated

出典と根拠

ORDレコード
ord-dfd893efca834bedb888dacd8689407d
出典データセット
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05008263

反応ノート

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