m-Chloroperbenzoic acid → HCID 86755926、化合物

HRID 366284ノート

反応式

HRID 366284 の反応式
[CH3:1][O:2][CH2:3][CH2:4]/[CH:5]=[CH:6]\[CH2:7][CH3:8].ClC1C=CC=C(C(OO)=[O:17])C=1>ClCCl>[CH2:7]([C@H:6]1[C@@H:5]([CH2:4][CH2:3][O:2][CH3:1])[O:17]1)[CH3:8]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 5364230(3Z)-1-Methoxy-3-hexene

生成物 1

HCID 86755926HCID 86755926、化合物収率 80%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

27.4 g of (Z)-1-methoxy-3-hexene were dissolved in dichloromethane (850 ml) and cooled to 10°. 62 g of ca 70% m-chloroperbenzoic acid corresponding to 1.05 eq., were added in portions. The mixture was allowed to react during 15 hours and was then transferred into an extraction funnel wherein it was washed with an aqueous solution of NaOH and then with water to neutrality. After separation and drying of the organic layer on Na2SO4, the residue was distilled over a 5 cm long Vigreux type column at 51-52°/1.5×103Pa to give 24.9 g (80%) of the desired compound in the form of a colourless liquid which presented the following analytical data:

後処理

  1. temperaturecooled to 10°
  2. customto react during 15 hours
  3. customwas then transferred into an extraction funnel
  4. washwherein it was washed with an aqueous solution of NaOH
  5. customAfter separation
  6. customdrying of the organic layer on Na2SO4
  7. distillationthe residue was distilled over a 5 cm long Vigreux type column at 51-52°/1.5×103Pa

出典と根拠

ORDレコード
ord-338e58e77cd24c89b0a9bce6c69402b7
出典データセット
uspto-grants-2000_10
特許番号
US06129941

反応ノート

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