Dichloromethane → Acequinocyl

HRID 1112137ノート

反応式

HRID 1112137 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-hydroxyl-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° C.) 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° C.)

出典と根拠

ORDレコード
ord-fbb9a6422dfc4d808f652233a750f4ee
出典データセット
uspto-grants-1978_10
特許番号
US04120897

反応ノート

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