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

HRID 270047ノート

反応式

HRID 270047 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-880336a7f2bd41f285555f722e87b84a
出典データセット
uspto-grants-2008_11
特許番号
US07449475B2

反応ノート

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