Lithium Hydroxide → HCID 68294980, 화합물

HRID 572523노트

반응식

HRID 572523 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12](=[O:19])[N:11]([CH3:20])[C:10]=1[C:21]([O:23]C)=[O:22].[OH-].[Li+]>O1CCCC1>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12](=[O:19])[N:11]([CH3:20])[C:10]=1[C:21]([OH:23])=[O:22]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 68295566HCID 68295566, 화합물

생성물 1

HCID 68294980HCID 68294980, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of methyl 4-(2,4-dimethylphenyl)-2-methyl-1-oxo-1,2-dihydroisoquinoline-3-carboxylate (30 g, 74.7 mmol) in tetrahydrofuran (THF) (400 mL) was treated with lithium hydroxide (8.94 g, 373 mmol) and stirred at reflux overnight. The mixture was concentrated and used crude in the next step (21.6 g, 94%). 1H NMR (400 MHz, DMSO-d6) δ ppm 13.81-14.14 (m, 1 H) 8.28-8.37 (m, 1 H) 7.62-7.69 (m, 1 H) 7.53-7.61 (m, 1 H) 7.13-7.19 (m, 1 H) 7.01-7.12 (m, 2 H) 6.82-6.91 (m, 1 H) 3.52 (s, 3 H) 2.34 (s, 3 H) 1.97 (s, 3 H); LC/MS (m/z) ES+=308 (M+1).

후처리

  1. temperatureat reflux overnight
  2. concentrationThe mixture was concentrated

출처 및 근거

ORD 기록
ord-3eb0f5a5d1f34de7831272b042b63493
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029391B2

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