Water → 4-Phenylmorpholin-3-ON

HRID 1817781

반응식

HRID 1817781 반응식
[NH:1]([CH2:8][CH2:9][OH:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.Cl[CH2:13][C:14](Cl)=[O:15].[OH-].[Na+]>C(O)C>[C:2]1([N:1]2[CH2:8][CH2:9][O:10][CH2:13][C:14]2=[O:15])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 14798Sodium HydroxideHCID 31235N-(2-Hydroxyethyl)aniline

생성물 1

HCID 51530804-Phenylmorpholin-3-ON

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
38 °C

실험 절차

In a 26-liter tank, 1.65 kg (12.0 mol) of 2-anilinoethanol are dissolved at room temperature in 1.53 l of ethanol and subsequently admixed with 4.58 l of water with stirring. The solution is heated to 38° C. 4.07 kg (3.0 equivalents) of chloroacetyl chloride and 6.60 kg of 45% sodium hydroxide solution (6.2 equivalents) are then added simultaneously at an internal temperature of 38 to 43° C. within 60 to 80 minutes, so that the pH is kept between 12 and 12.5. The mixture is stirred at a pH of 12 to 12.5 for 10 minutes, then cooled to 2° C. and stirred at this temperature for 30 minutes. The precipitated product is filtered off and washed twice with 3.3 kg each time of demineralized water at 2° C. The moist product is dried to constant mass at 50° C. under reduced pressure.

후처리

  1. stirringThe mixture is stirred at a pH of 12 to 12.5 for 10 minutes
  2. temperaturecooled to 2° C.
  3. stirringstirred at this temperature for 30 minutes
  4. filtrationThe precipitated product is filtered off
  5. washwashed twice with 3.3 kg each time of demineralized water at 2° C
  6. customThe moist product is dried to constant mass at 50° C. under reduced pressure

출처 및 근거

ORD 기록
ord-a9b7726ff18a492db93b7bb2fd6fe49b
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07598378B2

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