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2-Nitrobenzenesulfonyl chloride → HCID 117697629, 화합물

HRID 1778522
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HRID 1778522 반응식
Cl.[CH:2]12[NH:11][CH:6]([CH2:7][C:8](=[O:10])[CH2:9]1)[CH2:5][O:4][CH2:3]2.[N+:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[S:21](Cl)(=[O:23])=[O:22])([O-:14])=[O:13]>C(Cl)Cl>[N+:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[S:21]([N:11]1[CH:6]2[CH2:7][C:8](=[O:10])[CH2:9][CH:2]1[CH2:3][O:4][CH2:5]2)(=[O:23])=[O:22])([O-:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 155402-Nitrobenzenesulfonyl chlorideHCID 716271383-Oxa-9-azabicyclo[3.3.1]nonan-7-one--hydrogen chloride (1/1)

생성물 1

HCID 117697629HCID 117697629, 화합물수율 75%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 3-oxa-9-azabicyclo[3.3.1]nonan-7-one hydrochloride (CAS 1126795-00-3, 2.82 g), TEA (6.12 g, 60 mmol, 3.0 eq) and 2-Nitro-benzenesulfonyl chloride (8.84 g, 40 mmol, 2.0 eq) in DCM (100 mL) was stirred at room temperature for 10 h. Then the solvent was removed in vacuo, the residue was purified by silica gel (EA/PE=1:3) to give 9-(2-nitrophenyl)sulfonyl-3-oxa-9-azabicyclo[3.3.1]nonan-7-one 107b as a white solid, 4.90 g, yield: 75%. MS: calc'd (MH+) 327, measured (MH+) 327.

후처리

  1. customThen the solvent was removed in vacuo
  2. customthe residue was purified by silica gel (EA/PE=1:3)

출처 및 근거

ORD 기록
ord-875cb058775548bbb49fcd526d7a6658
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09266904B2

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