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

HRID 261476노트

반응식

HRID 261476 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 3.4 g of 2,3-dihydro-1'-acetyl-5-nitrospiro[benzofuran-2,4'-piperidine] in 150 ml of 6 N hydrochloric 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 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.

후처리

  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 removed
  5. customleaving a yellow residue
  6. customThe salt is collected
  7. customdried
  8. customfinally recrystallized twice from ethyl alcohol

출처 및 근거

ORD 기록
ord-122d54bf01484a2792bd4ac12456da3a
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166120

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