Triethylamine → HCID 72444859, 화합물

HRID 1767123노트

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HRID 1767123 반응식
C(N(CC)CC)C.Cl.[NH2:9][OH:10].[C:11]([C:13]12[N:19]([C:20]([O:22][CH2:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[O:21])[CH:16]([CH2:17][CH2:18]1)[CH2:15][CH2:14]2)#[N:12].[CH3:30][O:31][C:32]([C:34]#[C:35][C:36]([O:38][CH3:39])=[O:37])=[O:33]>CO>[CH3:30][O:31][C:32](=[O:33])[C:34]([O:10][N:9]=[C:11]([NH2:12])[C:13]12[N:19]([C:20]([O:22][CH2:23][C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)=[O:21])[CH:16]([CH2:17][CH2:18]1)[CH2:15][CH2:14]2)=[CH:35][C:36]([O:38][CH3:39])=[O:37]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 12980Dimethyl acetylenedicarboxylateHCID 443297Hydroxyamine hydrochlorideHCID 21112384Phenylmethyl 1-cyano-7-azabicyclo[2.2.1]heptane-7-carboxylate

생성물 1

HCID 72444859HCID 72444859, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Triethyl amine (1.5 eq.), hydroxylamine hydrochloride (1.3 eq.) were added to a solution of benzyl 1-cyano-7-azabicyclo[2.2.1]heptane-7-carboxylate (C-37) in absolute methanol. The mixture was stirred at room temperature overnight. The solvent was removed under reduced pressure, the residue was dissolved in chloroform and treated with dimethylacetylene dicarboxylate (2 eq.) for 14 hours at 60° C. The reaction mixture was then concentrated and the resulting crude oil was purified by flash chromatography (petroleum ether/EtOAc 1:1) to give the titled compound (C-38) as a mixture of isomers.

후처리

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue was dissolved in chloroform
  3. concentrationThe reaction mixture was then concentrated
  4. customthe resulting crude oil was purified by flash chromatography (petroleum ether/EtOAc 1:1)

출처 및 근거

ORD 기록
ord-e6bfe532e0324573952020e64f9ed5dc
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07232819B2

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