Triethylamine → HCID 19805452, 화합물

HRID 1681687

반응식

HRID 1681687 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19805452HCID 19805452, 화합물수율 37.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c97633e1fc2e4621b1f03bd0f273c36e
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05173496

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