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Formic Acid → HCID 22392274, 화합물

HRID 1358171
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HRID 1358171 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 284Formic AcidHCID 712FormaldehydeHCID 14798Sodium HydroxideHCID 21951121HCID 21951121, 화합물

생성물 1

HCID 22392274HCID 22392274, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 1140
Toluene
용매
HCID 64052-Methyl-2-butanol용매2회

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d57e964a13aa4eb9be8c74a42e16f220
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06596461B1

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