Triethylamine → HCID 19805452、化合物

HRID 1681687

反応式

HRID 1681687 の反応式
[C:1]([N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[NH:7]1)([O:3][CH2:4][CH3:5])=[O:2].C(N(CC)CC)C.Br[CH:24]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(Cl)(Cl)Cl>[C:1]([N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8](=[O:15])[N:7]1[CH:24]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([O:3][CH2:4][CH3:5])=[O:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 236603BromodiphenylmethaneHCID 584113Ethyl 3-oxo-2,3-dihydro-1H-indazole-1-carboxylate

生成物 1

HCID 19805452HCID 19805452、化合物収率 37.6%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 1,2-dihydro-1-carboethoxy-3H-indazol-3-one (G. Heller and P. Jacobsohn, Chem. Ber, 1921, 54B, 1107; 2.06 g), triethylamine (1.01 g) and bromodiphenylmethane (2.5 g) in chloroform (60 ml) was heated under reflux for 4 hours. The reaction mixture was then washed successively with water, M hydrochloric acid and then with water, dried (MgSO4) and evaporated. The residue was dissolved in methylene chloride and purified by column chromatography using an increasing gradient of ether in methylene chloride as eluant to give (from the later fractions) 1,2-dihydro-1-carboethoxy-2-diphenylmethyl-3H-indazol-3-one as a solid (1.4 g), m.p. 115-118° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. washThe reaction mixture was then washed successively with water, M hydrochloric acid
  4. dry with materialwith water, dried (MgSO4)
  5. customevaporated
  6. dissolutionThe residue was dissolved in methylene chloride
  7. custompurified by column chromatography

出典と根拠

ORDレコード
ord-c97633e1fc2e4621b1f03bd0f273c36e
出典データセット
uspto-grants-1992_12
特許番号
US05173496

関連ノート

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