Oxalic acid dihydrate → HCID 178513484、化合物

HRID 477768ノート

反応式

HRID 477768 の反応式
[C:1]([C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH2:9][CH2:10]2)=[C:5]([N+:13]([O-])=O)[C:4]=1[N+:16]([O-])=O)#[N:2].[OH2:19].O.[C:21](O)(=[O:25])[C:22](O)=[O:23]>C(O)C.[Pd]>[C:1]([C:3]1[C:4]2[N:16]=[C:22]([OH:23])[C:21]([OH:25])=[N:13][C:5]=2[C:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C:11]=2[CH:12]=1)(=[O:19])[NH2:2]

参加物

5

反応物 2

HCID 61373Oxalic acid dihydrateHCID 15066366HCID 15066366、化合物

生成物 1

HCID 178513484HCID 178513484、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of 7-cyano-1,2,3,4-tetrahydro-5,6-dinitro-naphthalene (0.18 g, 0.73 mmol) in ethanol was hydrogenated at room temperature and atmospheric pressure in the presence of 100 mg of 5% palladium-on-charcoal. The catalyst was filtered off, and the filtrate was evaporated to dryness. The solid residue was suspended in 10 ml of 1M hydrochloric acid, oxalic acid dihydrate (0.15 g, 1.2 mmol) was added, and the mixture was refluxed for 3 h. After cooling, the solid was collected and washed with water, ethanol and ether affording 80 mg (42%) of the amide.

後処理

  1. customwas hydrogenated at room temperature
  2. filtrationThe catalyst was filtered off
  3. customthe filtrate was evaporated to dryness
  4. temperaturethe mixture was refluxed for 3 h
  5. temperatureAfter cooling
  6. customthe solid was collected
  7. washwashed with water, ethanol and ether affording 80 mg (42%) of the amide

出典と根拠

ORDレコード
ord-0180999db6264b4ba6caae35547e36b2
出典データセット
uspto-grants-1989_12
特許番号
US04889855

反応ノート

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