Chlorosuccinimide → HCID 70579239, 화합물

HRID 1414570노트

반응식

HRID 1414570 반응식
[ClH:1].[CH3:2][N:3]1[CH2:8][CH2:7][C:6]2([C:21]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[O:15][C:14]3[C:9]2=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH2:5][CH2:4]1.[Cl:22]N1C(=O)CCC1=O>ClCCl>[ClH:22].[Cl:1][C:11]1[CH:12]=[CH:13][C:14]2[O:15][C:16]3[C:21]([C:6]4([CH2:7][CH2:8][N:3]([CH3:2])[CH2:4][CH2:5]4)[C:9]=2[CH:10]=1)=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3

참가 물질

4

반응물 2

HCID 31398ChlorosuccinimideHCID 14570249HCID 14570249, 화합물

생성물 1

HCID 70579239HCID 70579239, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1'-methylxanthene-9-spiro-4'-piperidine hydrochloride (5 g.), N-chlorosuccinimide (4.5 g.) and dichloromethane (100 ml.) is refluxed for 72 hours. The solution is washed with saturated sodium bicarbonate solution then water and dried with MgS04. The solution is evaporated to give a gummy residue which is chromatographed on grade 3 aluminium oxide, Woelm basic. The product is eluted with 30% petroleum-ether (b.p. 60°-80° C.)/chloroform, taken up in ether and the solution treated with ethereal hydrochloric acid. The precipitate is filtered and recrystallised from ethanol-ether to give 2,7-dichloro-1'-methylxanthene-9-spiro-4'-piperidine hydrochloride, m.p. 285° C.

후처리

  1. temperatureis refluxed for 72 hours
  2. washThe solution is washed with saturated sodium bicarbonate solution
  3. dry with materialwater and dried with MgS04
  4. customThe solution is evaporated
  5. customto give a gummy residue which
  6. customis chromatographed on grade 3 aluminium oxide, Woelm basic
  7. washThe product is eluted with 30% petroleum-ether (b.p. 60°-80° C.)/chloroform
  8. additionthe solution treated with ethereal hydrochloric acid
  9. filtrationThe precipitate is filtered
  10. customrecrystallised from ethanol-ether

출처 및 근거

ORD 기록
ord-c02a14a100ae4b90a748002859301f20
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001419

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