Water → HCID 19960978, 화합물

HRID 53880노트

반응식

HRID 53880 반응식
[CH2:1]([N:8]1[CH2:15][C:14]2([C:16]#[N:17])[CH:10]([CH2:11][O:12][CH2:13]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:17][CH2:16][C:14]12[CH2:15][N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[CH2:9][CH:10]1[CH2:11][O:12][CH2:13]2

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 19960963HCID 19960963, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19960978HCID 19960978, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

3.7 g (15.9 mmol) of 7-benzyl-1-cyano-3-oxa-7-azabicyclo[3.3.0]octane in 5 ml of absolute tetrahydrofuran are added dropwise to a mixture of 1.5 g of lithium aluminium hydride in 100 ml of absolute tetrahydrofuran and the resulting mixture is heated under reflux for 15 hours. Decomposition is effected with 1.5 ml each of water, 15% strength sodium hydroxide solution, and again water, and the mixture is filtered with suction, and the aluminium salts are extracted by boiling on two occasions with 100 ml of tetrahydrofuran. The tetrahydrofuran solutions are concentrated and the residue is distilled. Yield: 3.2 g (86% of theory) Boiling point: 125°-130° C./0.04 mbar

후처리

  1. temperaturethe resulting mixture is heated
  2. temperatureunder reflux for 15 hours
  3. filtrationthe mixture is filtered with suction
  4. extractionthe aluminium salts are extracted
  5. concentrationThe tetrahydrofuran solutions are concentrated
  6. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-d37da7198475475b83000f1d89aa6a2d
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05621105

반응 노트

불러오는 중…