Hydrochloric Acid → 2,3-Dihydro-5-nitrospiro[benzofuran-2,4'-piperidine]hydrochloride

HRID 261506ノート

反応式

HRID 261506 の反応式
C([N:4]1[CH2:9][CH2:8][C:7]2([CH2:13][C:12]3[CH:14]=[C:15]([N+:18]([O-:20])=[O:19])[CH:16]=[CH:17][C:11]=3[O:10]2)[CH2:6][CH2:5]1)(=O)C.[ClH:21]>CCOCC>[ClH:21].[N+:18]([C:15]1[CH:16]=[CH:17][C:11]2[O:10][C:7]3([CH2:6][CH2:5][NH:4][CH2:9][CH2:8]3)[CH2:13][C:12]=2[CH:14]=1)([O-:20])=[O:19]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 127332352,3-Dihydro-1'-acetyl-5-nitrospiro[benzofuran-2,4'-piperidine]

生成物 1

HCID 203942712,3-Dihydro-5-nitrospiro[benzofuran-2,4'-piperidine]hydrochloride

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A solution of 3.4 g of 2,3-dihydro-1'-acetyl-5-nitrospiro[benzofuran-2,4'-piperidine] in 150 ml of 6 N hydrochoric acid is refluxed for 45 hours and then stirred at ambient temperature for 16 hours. Thereafter, the reaction mixture is successively extracted once with ether, basified with 6 N sodium hydroxide and extracted thrice with ether. The combined ether extracts are dried and the solvent is removed, leaving a yellow residue. The residue is dissolved in ether where it is converted to its hydrogen chloride salt. The salt is collected, dried and finally recrystallized twice from ethyl alcohol to give the product, 2,3-dihydro-5-nitrospiro[benzofuran-2,4'-piperidine]hydrochloride, mp 265°-266° C.

後処理

  1. extractionThereafter, the reaction mixture is successively extracted once with ether
  2. extractionextracted thrice with ether
  3. dry with materialThe combined ether extracts are dried
  4. customthe solvent is removed
  5. customleaving a yellow residue
  6. customThe salt is collected
  7. customdried
  8. customfinally recrystallized twice from ethyl alcohol

出典と根拠

ORDレコード
ord-542513ba06184051839d480704a114b4
出典データセット
uspto-grants-1979_08
特許番号
US04166119

反応ノート

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