Dichloromethane → Acequinocyl

HRID 972886ノート

反応式

HRID 972886 の反応式
[CH2:1]([C:13]1[C:14](=[O:25])[C:15]2[C:20]([C:21](=[O:24])[C:22]=1[OH:23])=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C(N(CC)CC)C.[C:33](Cl)(=[O:35])[CH3:34].C(Cl)Cl>O>[C:33]([O:23][C:22]1[C:21](=[O:24])[C:20]2[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=2)[C:14](=[O:25])[C:13]=1[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])(=[O:35])[CH3:34]

参加物

6

反応物 4

HCID 6344Dichloromethane2 回HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 178442823HCID 178442823、化合物

生成物 1

HCID 93315Acequinocyl

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2.0 parts of 2-n-dodecyl-3-hydroxy-1,4-naphthoquinone, 0.81 parts of triethylamine, 0.63 parts of acetyl chloride and 50 parts of methylene chloride was stirred at room temperature for 30 hours. The resulting mixture was distributed between methylene chloride and water. The methylene chloride layer was separated, dried over magnesium sulfate, then filtered and evaporated under reduced pressure. The residue was crystallized from petroleum ether (b.p. 30°-60°) to give 1.2 parts of 3-acetoxy-2-n-dodecyl-1,4-naphthoquinone, m.p.57°-58° C.

後処理

  1. customThe methylene chloride layer was separated
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe residue was crystallized from petroleum ether (b.p. 30°-60°)

出典と根拠

ORDレコード
ord-44d6bb169e884b3f8a2bc6c5ce93c173
出典データセット
uspto-grants-1977_10
特許番号
US04053634

反応ノート

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