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m-Chloroperbenzoic acid → 2-[2-[(6-Bromohexyl)oxy]ethyl]pyridine N-oxide

HRID 2108043
ノート
印刷プレビュー

反応式

HRID 2108043 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[Br:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1>ClCCl>[Br:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][O:19][CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N+:23]=1[O-:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 151669352-(2-((6-Bromohexyl)oxy)ethyl)pyridine

生成物 1

HCID 538723032-[2-[(6-Bromohexyl)oxy]ethyl]pyridine N-oxide収率 92.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

m-Chloroperbenzoic acid (1.13 g) was added in one portion to a solution of 2-[2-[(6-bromohexyl)oxy]ethyl]pyridine (1.0 g) in dichloromethane (50 ml). The solution was stirred at room temperature overnight. The mixture was quenched with 10% w/v sodium sulphite solution (50 ml) and the organic layer washed with 8% sodium bicarbonate solution (50 ml). The organic layer was dried and evaporated to leave the title compound as a pale yellow oil (980 mg) used without further purification. A portion (100 mg) was purified by FCC eluting with System A (80:20:1) to give a pale yellow oil (20 mg), t.l.c. (System A 80:20:1) Rf 0.48.

後処理

  1. customThe mixture was quenched with 10% w/v sodium sulphite solution (50 ml)
  2. washthe organic layer washed with 8% sodium bicarbonate solution (50 ml)
  3. customThe organic layer was dried
  4. customevaporated

出典と根拠

ORDレコード
ord-87008fe0ad7145a5b223439de1f892ae
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04937251

反応ノート

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