Potassium Hydroxide → HCID 67491631、化合物

HRID 880972ノート

反応式

HRID 880972 の反応式
[CH3:1][O:2][C:3]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([O:14]C)=[O:13])=[CH:9][CH:10]=2)[N:5](C(OCC)=O)[N:4]=1.[OH-].[K+]>C(O)C>[CH3:1][O:2][C:3]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([OH:14])=[O:13])=[CH:9][CH:10]=2)[NH:5][N:4]=1

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 67491844HCID 67491844、化合物

生成物 1

HCID 67491631HCID 67491631、化合物収率 76%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

1-Ethyl 6-methyl 3-methoxy-1H-indazole-1,6-dicarboxylate (444 mg, 1.60 mmol) was suspended in ethanol (5 mL). An aqueous solution of potassium hydroxide (16 mL, 16 mmol, 1 M) was added and the reaction was heated to 65° C. and stirred for 1.5 hours. The reaction was cooled to room temperature and concentrated. The residue was taken up in water and the solution was acidified with 1 N aqueous hydrochloric acid until a precipitate formed. The solid was collected by filtration, rinsed with water, and dried under vacuum to give the title compound (232 mg, 76%) as an orange solid. +ESI (M+H) 193.2; 1H NMR (400 MHz, DMSO-d6, δ): 12.22 (s, 1H), 7.90-7.94 (m, 1H), 7.64 (d, J=8.4 Hz, 1H), 7.53 (dd, J=8.4, 1.4 Hz, 1H), 3.99 (s, 3H).

後処理

  1. temperatureThe reaction was cooled to room temperature
  2. concentrationconcentrated
  3. customformed
  4. filtrationThe solid was collected by filtration
  5. washrinsed with water
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-79971be39b87460082fe32bdb4d540d5
出典データセット
uspto-grants-2015_03
特許番号
US08993586B2

反応ノート

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