Cyclobutanone → tert-Butyl cyclobutylidenecarbazate

HRID 12918

반응식

HRID 12918 반응식
[C:1]1(=O)[CH2:4][CH2:3][CH2:2]1.[C:6]([O:10][C:11]([NH:13][NH2:14])=[O:12])([CH3:9])([CH3:8])[CH3:7]>CCCCCC>[C:6]([O:10][C:11]([NH:13][N:14]=[C:1]1[CH2:4][CH2:3][CH2:2]1)=[O:12])([CH3:9])([CH3:8])[CH3:7]

참가 물질

4

반응물 2

HCID 14496CyclobutanoneHCID 70091tert-Butyl carbazate

생성물 1

HCID 45092398tert-Butyl cyclobutylidenecarbazate수율 81.2%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

The reaction mixture of cyclobutanone (15 g, 214 mmol) and hydrazinecarboxylic acid tert-butyl ester (28.3 g, 214 mmol) in hexane (225 mL) was heated to reflux for 2 hours. After cooling down, a precipitate formed and the solid was filtered under vacuum. Isopropanol (10 mL) and hexane (100 mL) were added to the solid and the mixture was put on the rotary evaporator under vacuum until a slurry was generated. After filtration, the solid was washed with hexane twice and dried in vacuo to afford N′-cyclobutylidene-hydrazinecarboxylic acid tert-butyl ester (32 g, 81%) as white solid which was used without further purification.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 hours
  3. temperatureAfter cooling down
  4. customa precipitate formed
  5. filtrationthe solid was filtered under vacuum
  6. additionIsopropanol (10 mL) and hexane (100 mL) were added to the solid
  7. customthe mixture was put on the rotary evaporator under vacuum until a slurry
  8. filtrationAfter filtration
  9. washthe solid was washed with hexane twice
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-8077ea87bc5b4e968bb24e3cbfde846c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728029B2

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