Hydroxylamine → HCID 178526327、化合物

HRID 464646ノート

反応式

HRID 464646 の反応式
[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

参加物

6

反応物 4

HCID 787HydroxylamineHCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 21998189HCID 21998189、化合物

生成物 1

HCID 178526327HCID 178526327、化合物収率 30.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-ddf96b98a2af4e469092a249ac9243f2
出典データセット
uspto-grants-1985_10
特許番号
US04548929

反応ノート

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