1-Bromooctane → HCID 20322535、化合物

HRID 840003ノート

反応式

HRID 840003 の反応式
[K].[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[NH:8][C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3].[CH2:21](Br)[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]>CN(C)C=O>[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[N:8]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3]

参加物

5

反応物 3

HCID 81401-BromooctaneHCID 5462222PotassiumHCID 203401897,9-Diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione2 回

生成物 1

HCID 20322535HCID 20322535、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To 70 ml of dimethylformamide were added 8 g of the potassium salt of 7,9-diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione (Compound 1) and 5.2 g of octyl bromide; the mixture was heated, with stirring, at 60° C for 2 hours. The reaction mixture was then concentrated by evaporation under reduced pressure, and benzene was added to the residue. The resulting benzene solution was washed with water and then dried over magnesium sulphate. After removing the benzene, the resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine) and then by recrystallization from hexane, giving 3.0 g of Compound 5, mp 65° - 67° C.

後処理

  1. temperaturethe mixture was heated
  2. concentrationThe reaction mixture was then concentrated by evaporation under reduced pressure, and benzene
  3. additionwas added to the residue
  4. washThe resulting benzene solution was washed with water
  5. dry with materialdried over magnesium sulphate
  6. customAfter removing the benzene
  7. customthe resulting oily product was first purified by column chromatography on silica gel (eluent: benzene containing 5% of triethylamine)
  8. customby recrystallization from hexane

出典と根拠

ORDレコード
ord-a113adb3b1af40ceb38cfcd397f3a084
出典データセット
uspto-grants-1978_06
特許番号
US04097587

反応ノート

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