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Sodium Hydroxide → 4,5,6,7-Tetrahydro-1H-indazole-3-carboxylic acid

HRID 2182386
ノート
印刷プレビュー

反応式

HRID 2182386 の反応式
C([O:3][C:4]([C:6]1[C:14]2[CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[NH:8][N:7]=1)=[O:5])C.[OH-].[Na+]>CO>[NH:8]1[C:9]2[CH2:10][CH2:11][CH2:12][CH2:13][C:14]=2[C:6]([C:4]([OH:5])=[O:3])=[N:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 6624328ethyl 4,5,6,7-tetrahydro-1H-indazole-3-carboxylate

生成物 1

HCID 6488524,5,6,7-Tetrahydro-1H-indazole-3-carboxylic acid収率 81.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid ethyl ester [0.606 g, Reference Example 18(a)] in methanol (50 ml) was treated with sodium hydroxide (0.500 g). The mixture was refluxed for 16 hours, then cooled and then evaporated. The residual white solid was treated with hydrochloric acid (30 ml, 2N) and the resulting solution was extracted three times with ethyl acetate (50 ml). The combined organic extracts were dried over sodium sulfate and then evaporated to yield 4,5,6,7-tetrahydro-1H-indazole-3-carboxylic acid (0.424 g) as a white solid. LC-MS (METHOD B): RT=2.44 minutes; 167 (M+H)+. (b) 5-Isopropyl-1H-pyrazole-3-carboxylic acid

後処理

  1. temperatureThe mixture was refluxed for 16 hours
  2. temperaturecooled
  3. customevaporated
  4. additionThe residual white solid was treated with hydrochloric acid (30 ml, 2N)
  5. extractionthe resulting solution was extracted three times with ethyl acetate (50 ml)
  6. dry with materialThe combined organic extracts were dried over sodium sulfate
  7. customevaporated

出典と根拠

ORDレコード
ord-c077f266db1d498da2afc885b9036e05
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06897208B2

反応ノート

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