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Potassium Hydroxide → Ethylene glycol bis[2-hydroxy-3-(7,7,9,9-tetramethyl-2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propyl]ether

HRID 972030
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HRID 972030 반응식
[CH3:1][C:2]1([CH3:16])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11][C:4]2([NH:8][C:7](=[O:9])[NH:6][C:5]2=[O:10])[CH2:3]1.[O:17]1[CH2:28][CH:18]1[CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH:25]1[O:27][CH2:26]1.[OH-:29].[K+]>CO>[OH:17][CH:18]([CH2:28][N:6]1[C:5](=[O:29])[C:4]2([CH2:3][C:2]([CH3:1])([CH3:16])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11]2)[NH:8][C:7]1=[O:9])[CH2:19][O:20][CH2:21][CH2:22][O:23][CH2:24][CH:25]([OH:27])[CH2:26][N:6]1[C:5](=[O:10])[C:4]2([CH2:3][C:2]([CH3:16])([CH3:1])[NH:13][C:12]([CH3:15])([CH3:14])[CH2:11]2)[NH:8][C:7]1=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 16683Glycol diglycidyl etherHCID 12680667,7,9,9-Tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

생성물 1

HCID 131711586Ethylene glycol bis[2-hydroxy-3-(7,7,9,9-tetramethyl-2,4-dioxo-1,3,8-triazaspiro[4.5]dec-3-yl)propyl]ether

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 7.7 g of 7,7,9,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione, 2.5 g of ethylene glycol bis(2,3-epoxypropyl)ether and 0.1 g of potassium hydroxide in 80 ml of methanol was refluxed for 11 hours. Insoluble materials were then filtered off and the filtrate was washed with hot methanol. The solution was dried and then the solvent evaporated off. The residue was recrystallised from N,N-dimethylformamide, giving the desired compound in the form of white crystals, melting at 262°-264° C.

후처리

  1. temperaturewas refluxed for 11 hours
  2. filtrationInsoluble materials were then filtered off
  3. washthe filtrate was washed with hot methanol
  4. customThe solution was dried
  5. customthe solvent evaporated off
  6. customThe residue was recrystallised from N,N-dimethylformamide

출처 및 근거

ORD 기록
ord-8cdc1f6f705c4407b4c0af05e71bd929
출처 데이터셋
uspto-grants-1979_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04162246

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