Hydroxylamine → HCID 178526327, 화합물

HRID 2295292노트

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HRID 2295292 반응식
[NH2:1][OH:2].Cl.NO.C(=O)([O-])[O-].[Na+].[Na+].S([C:22]1[CH:27]2[CH2:28][CH:24]([CH:25]=[CH:26]2)[N:23]=1)(C1C=CC(C)=CC=1)(=O)=O>O1CCCC1>[CH:24]12[CH2:28][CH:27]([CH:26]=[CH:25]1)[C:22](=[N:1][OH:2])[NH:23]2

참가 물질

6

반응물 4

HCID 787HydroxylamineHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 21998189HCID 21998189, 화합물

생성물 1

HCID 178526327HCID 178526327, 화합물수율 30.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
25 °C

실험 절차

To a solution of hydroxylamine (from 2.1 g (0.03 m) of hydroxylamine hydrochloride, 4.3 g (0.015 m) of sodium carbonate, 10 ml of water and 200 ml of tetrahydrofuran) at 0° C. was added 5.16 g (0.021 m) of 3-tosyl-2-azabicyclo[2.2.1]hepta-2,5-diene (prepared by the procedure of J. Organic Chemistry, 39, 564 (1974)) in 50 ml of tetrahydrofuran. After being stirred overnight, during which time the temperature was allowed to warm to 25° C., the organic layer was separated, dried, and stripped of solvent. Purification of the residue by chromatography (silica gel: 1:1::dichloromethane:ethyl acetate) gave 0.8 g of material whose spectra were consistent with the title structure.

후처리

  1. customprepared by the procedure of J
  2. customthe organic layer was separated
  3. customdried
  4. customPurification of the residue by chromatography (silica gel: 1:1::dichloromethane:ethyl acetate)

출처 및 근거

ORD 기록
ord-3ea549eb93884441a194f4a070650edc
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04424213

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