1,3-Dibromopropane → HCID 54351699、化合物

HRID 27066ノート

反応式

HRID 27066 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH3:7][C:8]1[CH:9]=[C:10]([CH:24]=[C:25]([CH3:28])[C:26]=1[OH:27])[C:11]([C:13]1[O:14][C:15]2[C:20]([C:21](=[O:23])[CH:22]=1)=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:12].[Br:29][CH2:30][CH2:31][CH2:32]Br>CN(C)C=O>[Br:29][CH2:30][CH2:31][CH2:32][O:27][C:26]1[C:25]([CH3:28])=[CH:24][C:10]([C:11]([C:13]2[O:14][C:15]3[C:20]([C:21](=[O:23])[CH:22]=2)=[CH:19][CH:18]=[CH:17][CH:16]=3)=[O:12])=[CH:9][C:8]=1[CH3:7]

参加物

5

反応物 3

HCID 80011,3-DibromopropaneHCID 11430Potassium CarbonateHCID 64555162-(4-Hydroxy-3,5-dimethylbenzoyl)-4-benzopyrone

生成物 1

HCID 54351699HCID 54351699、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

27.6 g (0.2 mol) of potassium carbonate was added to a solution of 29.4 g (0.1 mol) of 2-(3,5-dimethyl 4-hydroxy benzoyl) chromone in 150 ml of dimethyl formamide, 101 g (0.5 mol) of 1,3-dibromo propane was added and the admixture left at ambient temperature for 15 hours with constant agitation. The potassium bromide precipitate was filtered, the dimethyl formamide was concentrated in vacuo and the residue dissolved in 300 ml of water. Extraction was effected with 200 ml of methylene chloride, and precipitation was then effected by adding 200 ml of ether. The product was 36 g of 2-[4-(3-bromo propoxy) 3,5-dimethyl benzoyl] chromone.

後処理

  1. additionwas added
  2. filtrationThe potassium bromide precipitate was filtered
  3. concentrationthe dimethyl formamide was concentrated in vacuo
  4. dissolutionthe residue dissolved in 300 ml of water
  5. extractionExtraction
  6. customwas effected with 200 ml of methylene chloride, and precipitation
  7. additionby adding 200 ml of ether

出典と根拠

ORDレコード
ord-27d8c0d2087641c8b0183c2e60b2269a
出典データセット
uspto-grants-1980_09
特許番号
US04220645

反応ノート

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