Lithium Hydroxide → HCID 89451654, 화합물

HRID 526043

반응식

HRID 526043 반응식
[CH3:1][C:2]1[C:11]2[N:10]3[CH:12]=[CH:13][CH:14]=[C:9]3[C:8](=[O:15])[N:7]([CH2:16][C:17]([O:19]C)=[O:18])[C:6]=2[N:5]=[CH:4][CH:3]=1.[Li+].[OH-]>CO.O.C1COCC1>[CH3:1][C:2]1[C:11]2[N:10]3[CH:12]=[CH:13][CH:14]=[C:9]3[C:8](=[O:15])[N:7]([CH2:16][C:17]([OH:19])=[O:18])[C:6]=2[N:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 89451658Methyl 2-(1-methyl-6-oxopyrido[2,3-e]pyrrolo[1,2-a]pyrazin-5(6H)-yl)acetate

생성물 1

HCID 89451654HCID 89451654, 화합물수율 73%

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

Methyl 2-(1-methyl-6-oxopyrido[2,3-e]pyrrolo[1,2-a]pyrazin-5(6H)-yl)acetate (517 mg, 1.91 mmol) was dissolved in 20 mL of MeOH/H2O/THF (1:1:4). LiOH (68.5 mg, 2.86 mmol) was added. The mixture was stirred at room temperature for 16 hours. The solvents were removed and residue was dissolved in water, washed with ether, then neutralized with 2N HCl to pH=3. 356 mg (73%) white solid was obtained after filtration and dried under vacuum. 1H NMR (400 MHz, DMSO) δ 12.90 (s, 1H), 8.27-8.17 (m, 2H), 7.29-7.19 (m, 2H), 6.80 (dd, J=2.9, 3.9 Hz, 1H), 5.02 (s, 2H), 2.85 (s, 3H). 13C NMR (101 MHz, DMSO, APT) δ 169.8, 154.5, 143.1, 141.4, 135.9, 123.9, 123.3, 122.8, 119.5, 113.3, 112.7, 41.6, 22.2. HRMS (m/z): calcd for C13H12N3O3 (M+H) 258.0879. found 258.0894.

후처리

  1. customThe solvents were removed
  2. dissolutionresidue was dissolved in water
  3. washwashed with ether

출처 및 근거

ORD 기록
ord-5b470fee8d3647829d7ebdd2eea241df
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09345703B2

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