Hydroxyurea → HCID 178425012, 화합물

HRID 1484475

반응식

HRID 1484475 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 178425012HCID 178425012, 화합물수율 58%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 887Methanol용매

반응 조건

온도
-11 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7a2e6175695c4873bd703fc7e5ba2b7d
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422247B2

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