Hydrochloric Acid → ethyl N-(2,4,6-trimethylphenylacetyl)-piperidine-2-carboxylate

HRID 703754

反応式

HRID 703754 の反応式
[C:1]1([CH3:13])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[CH2:9][C:10](Cl)=[O:11].[NH:14]1[CH2:24][CH2:23][CH2:22][CH2:21][CH:15]1[C:16]([O:18][CH2:19][CH3:20])=[O:17].C(N(CC)CC)C.Cl>O1CCCC1>[CH3:13][C:1]1[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[CH2:9][C:10]([N:14]1[CH2:24][CH2:23][CH2:22][CH2:21][CH:15]1[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[O:11]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 27517Ethyl piperidine-2-carboxylateHCID 110307542,4,6-Trimethylbenzeneacetyl chloride

生成物 1

HCID 14883010ethyl N-(2,4,6-trimethylphenylacetyl)-piperidine-2-carboxylate収率 95.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

223 g (1.125 mol) of mesityleneacetyl chloride are added dropwise at 0° to 10° C. to 182 ml (1.157 mol) of ethyl pipecolinate and 162 ml (1.157 mol) of triethylamine in 1,200 ml of absolute tetrahydrofuran (THF), followed by stirring for 1 hour at room temperature. After the mixture has been stirred into 5 liters of ice water and 500 ml of 1 N HCl, the product is filtered off with suction, washed with water and dried in vacuo at 50° C. over P2O5. 342.3 g (95.2% of theory) of ethyl N-(2,4,6-trimethylphenylacetyl)-piperidine-2-carboxylate are obtained.

後処理

  1. filtrationthe product is filtered off with suction
  2. washwashed with water
  3. dry with materialdried in vacuo at 50° C. over P2O5

出典と根拠

ORDレコード
ord-193ecb6fe6c54afdaf079156e523890e
出典データセット
uspto-grants-1991_01
特許番号
US04985063

関連ノート

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