Benzylhydroxylamine → N-(2-methyl-3-tetrahydropyranyloxypropylidene)-benzylamine-N-oxide

HRID 329792ノート

反応式

HRID 329792 の反応式
[CH3:1][CH:2]([CH2:5][O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][O:8]1)[CH:3]=O.[CH2:13]([NH:20][OH:21])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Cl-].[Ca+2].[Cl-]>CCOCC>[CH3:1][CH:2]([CH2:5][O:6][CH:7]1[CH2:12][CH2:11][CH2:10][CH2:9][O:8]1)[CH:3]=[N+:20]([O-:21])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 2794173BenzylhydroxylamineHCID 5284359Calcium ChlorideHCID 108883772-Methyl-3-tetrahydropyranyloxypropanal

生成物 1

HCID 86743656N-(2-methyl-3-tetrahydropyranyloxypropylidene)-benzylamine-N-oxide収率 62.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

An etheral solution (1 ml) of 2-methyl-3-tetrahydropyranyloxypropanal (37.9 mg; 0.20 mmol) was added dropwise to a suspension of benzylhydroxylamine (28.7 mg; 0.23 mmol) and powdery calcium chloride (22.2 mg; 0.20 mmol) in ether (0.5 ml) at 0° C., and the resultant mixture was stirred for 1.5 hours. The reaction mixture was purified by TLC using ethyl acetate to give N-(2-methyl-3-tetrahydropyranyloxypropylidene)-benzylamine-N-oxide (34.9 mg; yield, 57%).

後処理

  1. customThe reaction mixture was purified by TLC

出典と根拠

ORDレコード
ord-68d277b2cc2e4d4398f4f42e20a20de1
出典データセット
uspto-grants-1990_01
特許番号
US04892961

反応ノート

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