Lithium → HCID 23044990、化合物

HRID 2107952ノート

反応式

HRID 2107952 の反応式
[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]

参加物

5

反応物 2

HCID 3028194LithiumHCID 23044986HCID 23044986、化合物

生成物 1

HCID 23044990HCID 23044990、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8909Butyl ether溶媒

反応条件

温度
99 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1008bfcf2e4343009632d27e32ecc48b
出典データセット
uspto-grants-1990_06
特許番号
US04937244

反応ノート

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