Lithium → HCID 23044990, 화합물

HRID 2107952노트

반응식

HRID 2107952 반응식
[Li].[N:2]([N:4]1[C:9]([CH3:11])([CH3:10])[CH2:8][O:7][CH2:6][C:5]1([CH3:13])[CH3:12])=O>O1CCCC1.C(OCCCC)CCC>[NH2:2][N:4]1[C:5]([CH3:13])([CH3:12])[CH2:6][O:7][CH2:8][C:9]1([CH3:11])[CH3:10]

참가 물질

5

반응물 2

HCID 3028194LithiumHCID 23044986HCID 23044986, 화합물

생성물 1

HCID 23044990HCID 23044990, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8909Butyl ether용매

반응 조건

온도
99 °C

실험 절차

About 20% of a solution of 5 g of lithium alanate in 50 ml of tetrahydrofuran is added dropwise to a heated solution of 17.2 g of 4-nitroso-3,3,5,5-tetramethylmorpholine in 50 ml of tetrahydrofuran and 100 ml of dibutyl ether. The tetrahydrofuran is distilled off and the internal temperature is increased to 99° C. The remainder of the lithium alanate solution is then added dropwise and the mixture is kept at 70° C. for a further hour. After the mixture has been cooled in an ice-bath, 10 ml of water and 10 ml of 15% strength sodium hydroxide solution are carefully added. After filtration with suction, the filtrate is extracted by shaking first with water and then with 100 ml of 1N hydrochloric acid. The aqueous HCl phase is then extracted by shaking once more with diethyl ether and used in the next stage.

후처리

  1. distillationThe tetrahydrofuran is distilled off
  2. additionThe remainder of the lithium alanate solution is then added dropwise
  3. waitthe mixture is kept at 70° C. for a further hour
  4. temperatureAfter the mixture has been cooled in an ice-bath
  5. addition10 ml of water and 10 ml of 15% strength sodium hydroxide solution are carefully added
  6. filtrationAfter filtration with suction
  7. extractionthe filtrate is extracted
  8. extractionThe aqueous HCl phase is then extracted
  9. stirringby shaking once more with diethyl ether

출처 및 근거

ORD 기록
ord-1008bfcf2e4343009632d27e32ecc48b
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04937244

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