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1,4-Dibromobutane → HCID 90410761, 화합물

HRID 1403726
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HRID 1403726 반응식
[C:1]1([NH:7][S:8]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br[CH2:20][CH2:21][CH2:22][CH2:23]Br.C([O-])([O-])=O.[Cs+].[Cs+]>CC(C)=O>[O:10]=[S:8]1(=[O:9])[N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:23][CH2:22][CH2:21][CH2:20][N:11]1[C:12]([O:13][C:14]([CH3:15])([CH3:17])[CH3:16])=[O:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80561,4-DibromobutaneHCID 10796Cesium carbonateHCID 405110Phenylaminosulfonyl carbamic acid tert-butylester

생성물 1

HCID 90410761HCID 90410761, 화합물수율 39%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
60 °C

실험 절차

To a solution of tert-butyl N-phenylsulfamoylcarbamate (2.0 g, 7.35 mmol) and 1,4-dibromobutane (1.6 g, 7.35 mmol) in acetone (30 mL) was added Cs2CO3 (7.2 g, 22.05 mmol) and the mixture was stirred at 60° C. for 48 hours. The reaction mixture was filtered and concentrated under reduced pressure to afford tert-butyl 1,1-dioxo-7-phenyl-1λ6,2,7-thiadiazepane-2-carboxylate as a yellow oil (860 mg, 39%). LCMS (ESI): m/z=271.1 [M−56+H]+.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0e2031cd5a8b494e8fc84b89a205b7cb
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08912219B2

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