Diisopropylethylamine → HCID 66834820, 화합물

HRID 2275226노트

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HRID 2275226 반응식
[OH:1][C@H:2]([CH2:28][OH:29])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[C:20](=[O:21])[C:19]3[C:18]4[C:13](=[C:14]([OH:24])[C:15]([C:22]#[N:23])=[CH:16][CH:17]=4)[NH:12][C:11]=3[C:10]([CH3:26])([CH3:25])[C:9]=2[CH:27]=1.[CH3:30][Si](C=[N+]=[N-])(C)C.C(N(C(C)C)CC)(C)C>CO.C(Cl)(Cl)Cl>[OH:1][C@H:2]([CH2:28][OH:29])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]2[C:20](=[O:21])[C:19]3[C:18]4[C:13](=[C:14]([O:24][CH3:30])[C:15]([C:22]#[N:23])=[CH:16][CH:17]=4)[NH:12][C:11]=3[C:10]([CH3:26])([CH3:25])[C:9]=2[CH:27]=1

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 167693TrimethylsilyldiazomethaneHCID 668349048-((R)-2,3-dihydroxy-propoxy)-4-hydroxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile

생성물 1

HCID 66834820HCID 66834820, 화합물수율 62%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

Under nitrogen atmosphere, 8-((R)-2,3-dihydroxy-propoxy)-4-hydroxy-6,6-dimethyl-11-oxo-6,11-dihydro-5H-benzo[b]carbazole-3-carbonitrile (Compound U8-4-2, 8.0 mg, 20.39 μmol) was dissolved in methanol (2.0 mL) and chloroform (2.00 mL), added with trimethylsilyldiazomethane (diethyl ether solution, 2 M, 15.3 μL, 30.58 μmol) and diisopropylethylamine (0.05 mL), and then stirred at room temperature for 31 hr. The residues obtained from the reaction solution after concentration under reduced pressure were purified by silica gel column chromatography (methanol/dichloromethane) to obtain the title compound (5.1 mg, 62%).

후처리

  1. customThe residues obtained from the reaction solution
  2. concentrationafter concentration under reduced pressure
  3. customwere purified by silica gel column chromatography (methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-448cb698fc5e46e4b3f68c279d0df9de
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126931B2

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