Cyclobutanone → tert-Butyl cyclobutylidenecarbazate

HRID 12918

反応式

HRID 12918 の反応式
[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]

参加物

4

反応物 2

HCID 14496CyclobutanoneHCID 70091tert-Butyl carbazate

生成物 1

HCID 45092398tert-Butyl cyclobutylidenecarbazate収率 81.2%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8077ea87bc5b4e968bb24e3cbfde846c
出典データセット
uspto-grants-2010_06
特許番号
US07728029B2

関連ノート

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