Sulfamide → Tert-butyl 4-sulfamoyl-1,4-diazepane-1-carboxylate

HRID 1024952노트

반응식

HRID 1024952 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[S:15](N)([NH2:18])(=[O:17])=[O:16]>O1CCOCC1>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([S:15](=[O:17])(=[O:16])[NH2:18])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 82267SulfamideHCID 2756058Tert-butyl 1,4-diazepane-1-carboxylate

생성물 1

HCID 67051265Tert-butyl 4-sulfamoyl-1,4-diazepane-1-carboxylate

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution of 1,4-Diazepane-1-carboxylic acid tert-butyl ester (3.16 g) in dioxane (40 ml) was added sulfamide (4.0 g) and the reaction mixture was then heated at reflux for 18 h. The reaction mixture was then reduced in vacuo and the residue partitioned between EtOAc (100 ml) and H2O (100 ml). The organics were separated and the aqueous layer was re-extracted with EtOAc (2×100 ml). Organics were combined, dried (MgSO4) and reduced in vacuo to give the subtitle compound as a white solid. Yield: 4.27 g

후처리

  1. temperaturethe reaction mixture was then heated
  2. temperatureat reflux for 18 h
  3. customthe residue partitioned between EtOAc (100 ml) and H2O (100 ml)
  4. customThe organics were separated
  5. extractionthe aqueous layer was re-extracted with EtOAc (2×100 ml)
  6. dry with materialdried (MgSO4)

출처 및 근거

ORD 기록
ord-31df86d366644453ba117502086ef8eb
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722883B2

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