Hydrochloric Acid → Benzyl 4-methylidenepyrazolidine-1-carboxylate

HRID 22667

反応式

HRID 22667 の反応式
C(OC([N:8]1[CH2:12][C:11](=[CH2:13])[CH2:10][N:9]1[C:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15])=O)(C)(C)C.S(Cl)(Cl)=O.Cl>CO>[CH2:17]([O:16][C:14]([N:9]1[CH2:10][C:11](=[CH2:13])[CH2:12][NH:8]1)=[O:15])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 12970152Benzyl tert-butyl 4-methylidenepyrazolidine-1,2-dicarboxylate

生成物 1

HCID 12970153Benzyl 4-methylidenepyrazolidine-1-carboxylate収率 97%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of crude 4-methylenepyrazolidine-1,2-dicarboxylic acid 1-benzyl ester 2-tert-butyl ester, 8, (30 g) in methanol (300 ml.) is added thionyl chloride dropwise at 0° C. The reaction is warmed to room temperature and stirred an additional 18 hours. Concentration of the reaction in vacuo affords a yellow oil which crystallizes upon standing to provide 23 g (97% yield) of the desired product as the HCl salt.

後処理

  1. customConcentration of the reaction in vacuo
  2. customaffords a yellow oil which
  3. customcrystallizes

出典と根拠

ORDレコード
ord-38ddfbcdcc454345a2a2f4edeccffcbc
出典データセット
uspto-grants-2005_02
特許番号
US06849627B2

関連ノート

読み込み中…