Ammonia → 4-(2-Fluorophenyl)-4-phenylbutanoicacid

HRID 358042

반응식

HRID 358042 반응식
[CH:1]1[CH:6]=[CH:5][C:4]([CH2:7][C:8]2[C:13]([F:14])=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.N.[Na].Br[CH2:18][CH2:19][C:20]([OH:22])=[O:21].Cl>CCOCC.[N+]([O-])([O-])=O.[Fe+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>[F:14][C:13]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[CH:7]([C:4]1[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=1)[CH2:18][CH2:19][C:20]([OH:22])=[O:21]

참가 물질

8

반응물 5

HCID 222Ammonia2회HCID 313Hydrochloric AcidHCID 115533-Bromopropionic acidHCID 1380532-FluorodiphenylmethaneHCID 5360545Sodium2회

생성물 1

HCID 204500254-(2-Fluorophenyl)-4-phenylbutanoicacid

시약·촉매·용매 2

HCID 25251Ferric nitrate촉매HCID 3283Diethyl Ether용매

실험 절차

100 g of 2-fluorodiphenylmethane are slowly added dropwise to a solution of sodiuum amide which has been prepared from 500 ml of liquid ammonia, 0.22 g of iron (III) nitrate and 13.2 g of sodium. After 10 minutes, a solution of 40.75 g of 3-bromopropionic acid in 500 ml of ether is added dropwise. After a further 15 minutes, the ammonia is allowed to distill off. The crystallized-out sodium salt of 4-(2-fluorophenyl)-4-phenylbutyric acid is filtered off and washed with ether. The free acid is obtained by treating the sodium salt with dilute hydrochloric acid, extracting the mixture with ether and evaporating the ethereal solution. There is obtained 4-(2-fluorophenyl)-4-phenylbutyric acid of melting point 105°.

후처리

  1. waitAfter a further 15 minutes
  2. distillationto distill off
  3. filtrationThe crystallized-out sodium salt of 4-(2-fluorophenyl)-4-phenylbutyric acid is filtered off
  4. washwashed with ether
  5. customThe free acid is obtained
  6. extractionextracting the mixture with ether
  7. customevaporating the ethereal solution

출처 및 근거

ORD 기록
ord-deef2fb43cb5454fa132c07bd98a3f18
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464300

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