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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
ノート
印刷プレビュー

反応式

HRID 972030 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8cdc1f6f705c4407b4c0af05e71bd929
出典データセット
uspto-grants-1979_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04162246

反応ノート

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