3-Chloro-1,2-propanediol → 2,3-Dihydroxypropyl-3-aminobenzotrifluoride

HRID 34432

반응식

HRID 34432 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:6][CH:7]=1.Cl[CH2:13][CH:14]([OH:17])[CH2:15][OH:16].C(=O)([O-])[O-].[Na+].[Na+]>C(OC(O)C)C>[OH:17][CH:14]([CH2:15][OH:16])[CH2:13][C:3]1[C:2]([NH2:1])=[CH:7][CH:6]=[CH:5][C:4]=1[C:8]([F:9])([F:10])[F:11]

참가 물질

5

반응물 3

HCID 72903-Chloro-1,2-propanediolHCID 73753-(Trifluoromethyl)anilineHCID 10340Sodium Carbonate

생성물 1

HCID 704243742,3-Dihydroxypropyl-3-aminobenzotrifluoride

시약·촉매·용매 1

HCID 101298981-Ethoxyethanol용매

실험 절차

In a two liter three necked flask equipped with mechanical stirrer, refluxing condenser and thermometer was added 322.2 gms (2.0 moles) of 3-aminobenzotrifluoride, 500 ml of ethoxyethanol solvent and 442.0 gms (4 moles) 1-chloro-2,3-propanediol. While this mixture was cooling, 205 gms (2.36 moles) of sodium carbonate was added keeping the temperature below 35° C. The mixture was then heated to reflux for 24 hours. Afterwards, the crude reaction mixture was filtered from the salt by-product. The salt was then washed several times with chloroform and these washings were combined with the filtrate. The solvent and chloroform was then removed under low vacuum and high vacuum to give 450.5 gms of the crude bis-2,3-dihydroxypropyl-3-aminobenzotrifluoride as a viscous dark oil.

후처리

  1. temperaturerefluxing condenser
  2. temperatureWhile this mixture was cooling
  3. customthe temperature below 35° C
  4. temperatureThe mixture was then heated
  5. temperatureto reflux for 24 hours
  6. customAfterwards, the crude reaction mixture
  7. filtrationwas filtered from the salt by-product
  8. washThe salt was then washed several times with chloroform
  9. customThe solvent and chloroform was then removed under low vacuum and high vacuum

출처 및 근거

ORD 기록
ord-c708e6e536f34a48971a856e4648a83a
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761502

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