Hydroxyurea → HCID 178425012、化合物

HRID 1484475

反応式

HRID 1484475 の反応式
[OH:1][NH:2][C:3]([NH2:5])=[O:4].[CH3:6][CH:7]([CH3:15])[CH2:8][C:9](=O)[CH2:10][C:11](=O)[CH3:12].[Cl-:16].[NH4+]>Cl.CO>[ClH:16].[CH3:12][C:11]1[N:5]=[C:3]([OH:4])[N+:2]([O-:1])=[C:9]([CH2:8][CH:7]([CH3:15])[CH3:6])[CH:10]=1

参加物

6

反応物 3

HCID 3657HydroxyureaHCID 25517Ammonium ChlorideHCID 763542,4-Heptanedione, 6-methyl-

生成物 1

HCID 178425012HCID 178425012、化合物収率 58%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

反応条件

温度
-11 °C

実験手順

0.20 mol (15.21 g) hydroxy urea were dissolved in 300 ml of M HCl, 300 ml of methanol were added, and 0.20 mol (28.44 g) 6-methyl-2,4-heptanedione were added dropwise while cooling at −12 to −10° C. The solution was allowed to warm slowly to room temperature and stirred over night, then evaporated to dryness. The residue was suspended with 200 ml of acetone, the mixture cooled to below 0° C. in an ice/ethanol bath, the solid filtered off and washed with a little ice-cold acetone. After drying 7.23 g of a product was obtained, which contained 58% of the title compound and 42% of the by-product ammonium chloride.

後処理

  1. additionwere added
  2. temperatureto warm slowly to room temperature
  3. customevaporated to dryness
  4. temperaturethe mixture cooled to below 0° C. in an ice/ethanol bath
  5. filtrationthe solid filtered off
  6. washwashed with a little ice-cold acetone
  7. dry with materialAfter drying 7.23 g of a product
  8. customwas obtained

出典と根拠

ORDレコード
ord-7a2e6175695c4873bd703fc7e5ba2b7d
出典データセット
uspto-grants-2016_08
特許番号
US09422247B2

関連ノート

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