Ethyl chloroformate → Ethyl 4-(cyanomethyl)piperidine-1-carboxylate

HRID 327031

反応式

HRID 327031 の反応式
C1(C[N:8]2[CH2:13][CH2:12][CH:11]([CH2:14][C:15]#[N:16])[CH2:10][CH2:9]2)C=CC=CC=1.Cl[C:18]([O:20][CH2:21][CH3:22])=[O:19]>O1CCCC1>[C:15]([CH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:9][CH2:10]1)#[N:16]

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 5624991-Benzylpiperidine-4-acetonitrile

生成物 1

HCID 18941011Ethyl 4-(cyanomethyl)piperidine-1-carboxylate収率 81.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 25 parts of 1-(phenylmethyl)-4-piperidineacetonitrile in 178 parts of tetrahydrofuran were added dropwise 37.97 parts of ethyl chloroformate at room temperature. The reaction mixture was stirred for 15 hours at room temperature and was then evaporated. The residue was taken up in 90 parts of ethyl acetate and the whole was washed successively with HCl 3N, NaHCO3 and NaCl (sat.). The solvent was evaporated and the residue was distilled (100°-110° C./6.7 Pa), yielding 18.7 parts (81.4%) of ethyl 4-(cyanomethyl)-1-piperidinecarboxylate (interm. 24).

後処理

  1. customwas then evaporated
  2. washthe whole was washed successively with HCl 3N, NaHCO3 and NaCl (sat.)
  3. customThe solvent was evaporated
  4. distillationthe residue was distilled (100°-110° C./6.7 Pa)

出典と根拠

ORDレコード
ord-6231955ae036458fa3203c65f9c0214e
出典データセット
uspto-grants-1993_12
特許番号
US05272150

関連ノート

読み込み中…