Chlorosuccinimide → HCID 70579239、化合物

HRID 1414570ノート

反応式

HRID 1414570 の反応式
[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

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 14570249HCID 14570249、化合物

生成物 1

HCID 70579239HCID 70579239、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c02a14a100ae4b90a748002859301f20
出典データセット
uspto-grants-1977_01
特許番号
US04001419

反応ノート

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