Methanol → HCID 178487707, 화합물

HRID 1367727노트

반응식

HRID 1367727 반응식
[Cl:1][C:2]1[C:3]([O:17][CH3:18])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:12]([O:14]C)=[O:13])[CH:8]=[C:7]2[OH:16].CO.C1COCC1.[Li+].[OH-]>O>[Cl:1][C:2]1[C:3]([O:17][CH3:18])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:12]([OH:14])=[O:13])[CH:8]=[C:7]2[OH:16]

참가 물질

6

반응물 4

HCID 887MethanolHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 178498513HCID 178498513, 화합물

생성물 1

HCID 178487707HCID 178487707, 화합물수율 99.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of methyl 8-chloro-4-hydroxy-7-methoxyquinoline-2-carboxylate (36.5 g, 0.145 mol) in a mixture of 1:1 of MeOH: THF (160 mL total) was added a solution of LiOH (30.5 g, 0.725 mol) in H2O (80 mL). The mixture was stirred at room temperature for an hour when LCMS analysis showed complete conversion to the carboxylic acid. The reaction was worked up by removal of the volatiles and adjusting the pH of the solution to 6 using aqueous 6N HCl. The resulted gummy residue was filtered and dried on the lypholizer for 2 days to provide 34.4 g (99.6%) of the product as a white solid. EI MS (m/z) 253.9 [M+H].

후처리

  1. customThe reaction was worked up by removal of the volatiles
  2. filtrationThe resulted gummy residue was filtered
  3. customdried on the lypholizer for 2 days

출처 및 근거

ORD 기록
ord-c01d9888568a487d8d3ee55e0f2a4807
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893264B2

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