Lithium Hydroxide → 2-Carboxy-6-chloro-7-methyl-4-oxoquinoline

HRID 6681

반응식

HRID 6681 반응식
C[O:2][C:3]([C:5]1[CH2:14][C:13](=[O:15])[C:12]2[C:7](=[CH:8][C:9]([CH3:17])=[C:10]([Cl:16])[CH:11]=2)[N:6]=1)=[O:4].[OH-].[Li+]>CO.O>[C:3]([C:5]1[CH2:14][C:13](=[O:15])[C:12]2[C:7](=[CH:8][C:9]([CH3:17])=[C:10]([Cl:16])[CH:11]=2)[N:6]=1)([OH:4])=[O:2]

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 684363462-Methoxycarbonyl-6-chloro-7-methyl-4-oxoquinoline

생성물 1

HCID 684353962-Carboxy-6-chloro-7-methyl-4-oxoquinoline수율 88.7%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

2-Methoxycarbonyl-6-chloro-7-methyl-4-oxoquinoline (7.00 g, 28.00 mmol) was suspended in 300 mL of MeOH and 100 mL of water. Lithium hydroxide (3.40 g, 90 mmol) was added and the reaction was stirred at room temp for 2 hours. The methanol was evaporated in vacuo and the product was crystallized by addition of 2N hydrochloric acid. The solid was filtered, washed with water and dried to afford 5.9 g (88%) of 2-carboxy-6-chloro-7-methyl-4-oxoquinoline: H NMR (DMSO-d6) 2.40 (s, 3), 6.60 (s, 1), 7.84 (s, 1), 7.98 (s, 1) ppm.

후처리

  1. customThe methanol was evaporated in vacuo
  2. customthe product was crystallized by addition of 2N hydrochloric acid
  3. filtrationThe solid was filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-11b76eafc4824bf4a143a7e2a8c5476d
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084142B2

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