m-Chloroperbenzoic acid → NY 4138

HRID 905232ノート

反応式

HRID 905232 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[S:12]1[CH:16]=[CH:15][CH:14]=[C:13]1[CH2:17][S:18][C:19]1[N:24]=[CH:23][C:22]([Br:25])=[CH:21][N:20]=1>ClCCl>[S:12]1[CH:16]=[CH:15][CH:14]=[C:13]1[CH2:17][S:18]([C:19]1[N:24]=[CH:23][C:22]([Br:25])=[CH:21][N:20]=1)=[O:9]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 20475699HCID 20475699、化合物

生成物 1

HCID 133258NY 4138収率 53%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

85% m-Chloroperbenzoic acid (1.5 mmol) was added to a solution of 2-(2-thienylmethylthio)-5-bromopyrimidine (1.5 mmol) in dichloromethane (25 ml) at -10° C. and the solution left at 0° C. for 18 h. The dichloromethane solution was then washed with saturated aqueous solutions of Na2SO and NaHCO3, and the dried (MgSO4) solution evaporated to leave the title compound; yield 53%, m.p. 108°-109° C. (iPrOH). 1H NMR (CDCl3) δ4.53 (CH2, 6.9 (H-3', H-4'), 7.16 (H-5'), 8.83 (H-4, H-6).

後処理

  1. washThe dichloromethane solution was then washed with saturated aqueous solutions of Na2SO and NaHCO3
  2. dry with materialthe dried (MgSO4) solution
  3. customevaporated

出典と根拠

ORDレコード
ord-8ca5d55e1db345b4930439a0518b6115
出典データセット
uspto-grants-1983_12
特許番号
US04423047

反応ノート

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