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

HRID 1903014노트

반응식

HRID 1903014 반응식
[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

참가 물질

6

반응물 4

HCID 241BenzeneHCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 13505937HCID 13505937, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e326b14dd8a44215accfb5ea883d9eb2
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04435322

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