Ethanol → HCID 136058092, 화합물

HRID 2077052노트

반응식

HRID 2077052 반응식
C(O)C.[Na].[Cl:5][C:6]1[CH:7]=[C:8]([CH2:12][C:13](=[NH:15])[NH2:14])[CH:9]=[CH:10][CH:11]=1.[CH2:16]([N:23]1[CH2:29][CH2:28][C:27](=O)[CH:26]([C:31](OCC)=[O:32])[CH2:25][CH2:24]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:16]([N:23]1[CH2:24][CH2:25][C:26]2[C:31](=[O:32])[NH:15][C:13]([CH2:12][C:8]3[CH:9]=[CH:10][CH:11]=[C:6]([Cl:5])[CH:7]=3)=[N:14][C:27]=2[CH2:28][CH2:29]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 5360545Sodium2회HCID 12485292Ethyl 1-benzyl-5-oxoazepane-4-carboxylateHCID 17221604(3-Chlorophenyl)ethanimidamide

생성물 1

HCID 136058092HCID 136058092, 화합물수율 33%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Ethanol (30 ml) was cooled in an ice bath then sodium (160 mg, 6.70 mmol) was added, with vigorous stirring. Once the sodium was dissolved, 2-(3-chlorophenyl)ethanimidamide (474 mg, 2.81 mmol) and ethyl 1-benzyl-5-oxoazepane-4-carboxylate (876 mg, 2.81 mmol) was added. The reaction mixture was refluxed, under nitrogen, for 17 h. Water (2 ml) was added to quench the reaction then the reaction mixture was concentrated in vacuo. The residue was partitioned between ethyl acetate (20 ml) and water (20 ml). The organic phase was dried over magnesium sulphate and concentrated in vacuo. Trituration of the residue with diethyl ether afforded the title compound as a solid in 33% yield, 361 mg.

후처리

  1. temperatureThe reaction mixture was refluxed, under nitrogen, for 17 h
  2. customto quench
  3. customthe reaction
  4. concentrationthe reaction mixture was concentrated in vacuo
  5. customThe residue was partitioned between ethyl acetate (20 ml) and water (20 ml)
  6. dry with materialThe organic phase was dried over magnesium sulphate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-d6030263b57c40c7aa24a41eaf67fb2c
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928099B2

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