m-Chloroperbenzoic acid → N-ethyl-3,6-carbazolediol diacetate

HRID 1580081ノート

反応式

HRID 1580081 の反応式
C([C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH2:20][CH3:21])[C:9]3[C:14]([C:15]=2[CH:16]=1)=[CH:13][C:12](C(=O)C)=[CH:11][CH:10]=3)(=O)C.ClC1C=CC=[C:25]([C:29]([O:31]O)=[O:30])C=1>C(Cl)(Cl)Cl>[C:29]([O:31][C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH2:20][CH3:21])[C:9]3[C:14]([C:15]=2[CH:16]=1)=[CH:13][C:12]([O:31][C:29](=[O:30])[CH3:25])=[CH:11][CH:10]=3)(=[O:30])[CH3:25]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 6220833,6-Diacetyl-9-ethylcarbazole

生成物 1

HCID 12331788N-ethyl-3,6-carbazolediol diacetate

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 104 g (0.37 mole) of 3,6-diacetyl-N-ethylcarbazole in 1700 ml of chloroform (hydrocarbon stabilized) previously cooled to 15°C was added 138 g (0.8 mole) of m-chloroperbenzoic acid. The reaction was stirred at room temperature for 4 days, then filtered. The filtrate was washed with saturated sodium bicarbonate solution and with water, then dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo leaving a solid which was recrystallized from acetone-water and then from acetone methanol to give the desired product. M.P. 138°-139°C, λmaxEtOH 237, E1cm1% 1330.

後処理

  1. filtrationfiltered
  2. washThe filtrate was washed with saturated sodium bicarbonate solution and with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customevaporated to dryness in vacuo
  5. customleaving a solid which
  6. customwas recrystallized from acetone-water

出典と根拠

ORDレコード
ord-b14c9664b0a8410e8bee4f203f097823
出典データセット
uspto-grants-1976_01
特許番号
US03932424

反応ノート

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