Benzene → HCID 15291091、化合物

HRID 128702

反応式

HRID 128702 の反応式
C1OCCOCCOCCOCCOCCOC1.C1C=CC=CC=1.Cl[CH2:26][N:27]1[C:37](=[O:38])[C:36]2[C:31](=[CH:32][C:33]([O:42][CH3:43])=[CH:34][C:35]=2[CH:39]([CH3:41])[CH3:40])[S:28]1(=[O:30])=[O:29].[N-:44]=[N+:45]=[N-:46].[Na+]>O>[N:44]([CH2:26][N:27]1[C:37](=[O:38])[C:36]2[C:31](=[CH:32][C:33]([O:42][CH3:43])=[CH:34][C:35]=2[CH:39]([CH3:41])[CH3:40])[S:28]1(=[O:30])=[O:29])=[N+:45]=[N-:46]

参加物

6

反応物 4

HCID 241BenzeneHCID 2855718-Crown-6HCID 33557Sodium AzideHCID 99951732-(Chloromethyl)-4-isopropyl-6-methoxybenzo[D]isothiazol-3(2H)-one 1,1-dioxide

生成物 1

HCID 15291091HCID 15291091、化合物収率 26%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 18-crown-6 ether (0.60 g) and benzene (60 mL) was heated under reflux with a water separator for 1 hour, then cooled to room temperature. 2-Chloromethyl-4-isopropyl-6-methoxysaccharin (3.03 g) and sodium azide (0.65 g) were added, and the mixture was stirred for a week at room temperature, then chromatographed on a column of silica gel (silica gel 60, 83 g) using benzene as eluant. The fractions containing the product, which were identified by thin layer chromatography, were combined and concentrated affording 2-azidomethyl-4-isopropyl-6-methoxysaccharin as a solution in benzene (250 mL).

後処理

  1. customchromatographed on a column of silica gel (silica gel 60, 83 g)
  2. additionThe fractions containing the product, which
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-1d4838076b604dfe911e87f95da97d89
出典データセット
uspto-grants-1995_11
特許番号
US05464852

関連ノート

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