Urea → 1,5-Dimethyl-4-phenylimidazolidin-2-one

HRID 902461

反応式

HRID 902461 の反応式
[CH3:1][C@H:2](NC)[C@H:3](O)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.S(=O)(=O)([O-])N.[NH4+].[NH2:19][C:20]([NH2:22])=[O:21].[CH3:23]N1C(=O)CCC1>O>[CH3:23][N:19]1[CH:2]([CH3:1])[CH:3]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:22][C:20]1=[O:21]

参加物

6

反応物 4

HCID 1176UreaHCID 9294EphedrineHCID 13387N-methyl-2-pyrrolidoneHCID 24482Ammonium sulfamate

生成物 1

HCID 2305471,5-Dimethyl-4-phenylimidazolidin-2-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
177.5 °C

実験手順

1 mol of an ephedrine, 1.025 mol of ammonium sulfamate, 3 mol of urea and the proton-donating compound were introduced into 200 ml of NMP. The reaction mixture was heated to 175 to 180° C. and stirred at this temperature for 2.5 h. It was then cooled to 130° C. and, at this temperature, water was added dropwise to the reaction mixture. Two phases formed. The lower phase was removed at 95° C. The upper phase was further cooled initially to 65° C. Crystals formed at this temperature. It was cooled further to 10° C. and stirred at this temperature for 1 h. The crystals were filtered off with suction and washed twice with cold water. The solid was dried in vacuo at RT overnight.

後処理

  1. additionwas added dropwise to the reaction mixture
  2. customTwo phases formed
  3. customThe lower phase was removed at 95° C
  4. temperatureThe upper phase was further cooled initially to 65° C
  5. customCrystals formed at this temperature
  6. temperatureIt was cooled further to 10° C.
  7. stirringstirred at this temperature for 1 h
  8. filtrationThe crystals were filtered off with suction
  9. washwashed twice with cold water
  10. customThe solid was dried in vacuo at RT overnight

出典と根拠

ORDレコード
ord-0c674f87262c463884a0803402d2a8e9
出典データセット
uspto-grants-2008_04
特許番号
US07365210B2

関連ノート

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