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Formic Acid → HCID 22392274、化合物

HRID 1358171
ノート
印刷プレビュー

反応式

HRID 1358171 の反応式
C=O.[OH:3][CH2:4][CH2:5][N:6]1[CH2:11][C:10]([CH3:13])([CH3:12])[NH:9][C:8]([CH3:15])([CH3:14])[C:7]1=[O:16].[CH:17](O)=O.[OH-].[Na+]>C(O)(CC)(C)C.O.C1(C)C=CC=CC=1>[OH:3][CH2:4][CH2:5][N:6]1[CH2:11][C:10]([CH3:12])([CH3:13])[N:9]([CH3:17])[C:8]([CH3:15])([CH3:14])[C:7]1=[O:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 21951121HCID 21951121、化合物

生成物 1

HCID 22392274HCID 22392274、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 1140
Toluene
溶媒
HCID 64052-Methyl-2-butanol溶媒2 回

反応条件

温度
80 °C

実験手順

24.3 g (0.78 mol) of paraformaldehyde are added to a solution of 120 g (0.6 mol) of 1-(2-hydroxyethyl)-3,3,5,5-tetramethylpiperazin-2-one in 300 ml of tert-amyl alcohol. The mixture is then heated to 80° C. and 35.8 g (0.78 mol) of formic acid dissolved in 30 ml of tert-amyl alcohol are slowly added. Then, the mixture is maintained at 80° C. for further 1 hour and cooled to 50° C. Subsequently, 250 ml of toluene and 100 ml of water are added. The mixture is then stirred and 33 g (0.825 mol) of sodium hydroxide dissolved in 60 ml of water are slowly added. The organic phase is separated, washed with water, dried over anhydrous sodium sulfate, filtered and evaporated under vacuum (60° C./10 mbar). A white solid with a melting point of 77°-80° C. is obtained.

後処理

  1. additionare slowly added
  2. temperatureThen, the mixture is maintained at 80° C. for further 1 hour
  3. temperaturecooled to 50° C
  4. additionare slowly added
  5. customThe organic phase is separated
  6. washwashed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customevaporated under vacuum (60° C./10 mbar)
  10. customA white solid with a melting point of 77°-80° C. is obtained

出典と根拠

ORDレコード
ord-d57e964a13aa4eb9be8c74a42e16f220
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06596461B1

反応ノート

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