Bromobenzene → HCID 13363395、化合物

HRID 867003ノート

反応式

HRID 867003 の反応式
[C:1]([N:4]1[CH2:12][CH2:11][CH:7]([C:8](Cl)=[O:9])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl-].[Al+3].[Cl-].[Cl-].[Br:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(Cl)CCl>[C:1]([N:4]1[CH2:12][CH2:11][CH:7]([C:8](=[O:9])[C:21]2[CH:22]=[CH:23][C:18]([Br:17])=[CH:19][CH:20]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 7961BromobenzeneHCID 1009501-Acetylpiperidine-4-carbonyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 13363395HCID 13363395、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

32.0 g of 1-acetylisonipecotoyl chloride, Example 1(b) are added portionwise to a stirred mixture of 45.3 g of aluminum chloride, 28.3 g of bromobenzene and 120 ml of ethylene dichloride. The solution is stirred overnight, poured onto ice, the organic phase is collected, and the aqueous layer is extracted with chloroform. The organic solutions are combined, dried, and the solvent is removed under reduced pressure to give a yellow oil which crystallizes to a soft solid. The solid is triturated with ether, collected and dried to give 1-acetyl-4-(4-bromobenzoyl)piperidine.

後処理

  1. additionpoured onto ice
  2. customthe organic phase is collected
  3. extractionthe aqueous layer is extracted with chloroform
  4. customdried
  5. customthe solvent is removed under reduced pressure
  6. customto give a yellow oil which
  7. customcrystallizes to a soft solid
  8. customThe solid is triturated with ether
  9. customcollected
  10. customdried

出典と根拠

ORDレコード
ord-409255d15f8b408fa08b756a4133c85f
出典データセット
uspto-grants-1978_07
特許番号
US04101663

反応ノート

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