Benzene → Diethyl 1-benzyl-4-oxoazetidine-2,2-dicarboxylate

HRID 1903014ノート

反応式

HRID 1903014 の反応式
[CH2:1]([N:8]([CH:13]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9](=[O:12])[CH2:10]Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.C1C=CC=CC=1.Cl>O>[CH2:1]([N:8]1[C:9](=[O:12])[CH2:10][C:13]1([C:19]([O:21][CH2:22][CH3:23])=[O:20])[C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 13505937HCID 13505937、化合物

生成物 1

HCID 13505935Diethyl 1-benzyl-4-oxoazetidine-2,2-dicarboxylate収率 75%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

34.1 g. (0.1 moles) of diethyl N-benzyl-N-(chloroacetyl)-amino-malonate prepared according to Example 19 and 18.2 ml. (13.2 g., 0.13 moles) of triethyl amine in 100 ml. of benzene are stirred at room temperature for 8 hours. The mixture is shaken with 100 ml. of water, 50 ml. of a 10% aqueous hydrochloric acid solution and again with 100 ml. of water. The organic phase is dried with magnesium sulfate, filtered and from the filtrate benzene is distilled off. The oily residue is distilled at 149° to 150° C., under a pressure of 0.1 mmHg. 23 g. (75%) of the named compound are obtained.

後処理

  1. dry with materialThe organic phase is dried with magnesium sulfate
  2. filtrationfiltered and from the filtrate benzene
  3. distillationis distilled off
  4. distillationThe oily residue is distilled at 149° to 150° C., under a pressure of 0.1 mmHg

出典と根拠

ORDレコード
ord-e326b14dd8a44215accfb5ea883d9eb2
出典データセット
uspto-grants-1984_03
特許番号
US04435322

反応ノート

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