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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 19814318、化合物

HRID 466612
ノート
印刷プレビュー

反応式

HRID 466612 の反応式
[CH3:1][NH2:2].[CH2:3]([N:10]1[CH2:21][CH2:20][C:13]2([O:17][C:16](=O)[O:15][C:14]2=[CH2:19])[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C(C)=CC=CC=1>[CH2:3]([N:10]1[CH2:21][CH2:20][C:13]2([O:17][C:16](=[O:15])[N:2]([CH3:1])[C:14]2=[CH2:19])[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6329MethylamineHCID 521998p-Toluenesulfonic acid monohydrateHCID 19814218HCID 19814218、化合物

生成物 1

HCID 19814318HCID 19814318、化合物収率 96.7%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒2 回

実験手順

A solution of 1.6 g of methylamine in 35 ml of xylene prepared at 0° C. is flown to the solution of 13.0 g of 8-benzyl-4-methylene-2-oxo-1,3-dioxa-8-azaspiro[4,5]decane in 30 ml of xylene under stirring. The reaction is exothermic, thus the temperature of the reaction mixture increases up to 55° to 60° C. Thereafter, the heterogeneous reaction mixture is heated to a temperature of 100° to 102° C., maintained at the same temperature for 10 minutes, then 0.2 g of p-toluenesulfonic acid monohydrate is added to the solution and the reaction mixture is boiled while the water formed in the reaction is azeotropically distilled out. After termination of the reaction the mixture is cooled down to room temperature, washed with 5% by weight aqueous sodium hydroxide solution and after separation the xylene phase is washed to neutral with water. The organic phase is dried over anhydrous sodium sulfate and evaporated under reduced pressure. The residue is recrystallized from a mixture of ethanol and diisopropyl ether under clarifying by activated carbon to obtain the title compound in 96.7% yield, m.p.: 96°-97° C.

後処理

  1. temperaturethus the temperature of the reaction mixture increases up to 55° to 60° C
  2. temperatureThereafter, the heterogeneous reaction mixture is heated to a temperature of 100° to 102° C.
  3. temperaturemaintained at the same temperature for 10 minutes
  4. customformed in the reaction
  5. distillationis azeotropically distilled out
  6. customAfter termination of the reaction the mixture
  7. washwashed with 5% by weight aqueous sodium hydroxide solution
  8. customafter separation the xylene phase
  9. washis washed to neutral with water
  10. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  11. customevaporated under reduced pressure
  12. customThe residue is recrystallized from a mixture of ethanol and diisopropyl ether under clarifying by activated carbon

出典と根拠

ORDレコード
ord-26bb43a778ec47d387b60ba84a8c2471
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05157038

反応ノート

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