1-Chloroethyl chloroformate → 6-Chlorospiro[chroman-2,4'-piperidine] hydrochloride

HRID 270047노트

반응식

HRID 270047 반응식
C([N:8]1[CH2:13][CH2:12][C:11]2([CH2:22][CH2:21][C:20]3[C:15](=[CH:16][CH:17]=[C:18]([Cl:23])[CH:19]=3)[O:14]2)[CH2:10][CH2:9]1)C1C=CC=CC=1.ClC(OC(Cl)C)=O>C1(C)C=CC=CC=1>[ClH:23].[Cl:23][C:18]1[CH:19]=[C:20]2[C:15](=[CH:16][CH:17]=1)[O:14][C:11]1([CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1)[CH2:22][CH2:21]2

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 598336421'-Benzyl-6-chloro-3,4-dihydrospiro[chromene-2,4'-piperidine]

생성물 1

HCID 689620726-Chlorospiro[chroman-2,4'-piperidine] hydrochloride수율 84.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 1′-benzyl-6-chloro-3,4-dihydrospiro[chromene-2,4′-piperidine] (1.63 g, 5.0 mmol) and 1-chloroethyl chloroformate (1.07 g, 7.5 mmol) in toluene (5 ml) was heated with reflux overnight. The solvent was removed i. vacuo, the oily residue dissolved in methanol (10 ml) and heated with reflux overnight. The solvent was removed in vacuo, and the residue treated with diethyl ether (50 ml). The white precipitate was collected by filtration, washed with diethyl ether and dried to afford the subtitle compound as white powder (0.58 g, 49%).

후처리

  1. temperaturewith reflux overnight
  2. customThe solvent was removed i
  3. dissolutionvacuo, the oily residue dissolved in methanol (10 ml)
  4. temperatureheated
  5. temperaturewith reflux overnight
  6. customThe solvent was removed in vacuo
  7. additionthe residue treated with diethyl ether (50 ml)
  8. filtrationThe white precipitate was collected by filtration
  9. washwashed with diethyl ether
  10. customdried

출처 및 근거

ORD 기록
ord-880336a7f2bd41f285555f722e87b84a
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449475B2

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