Hydrochloric Acid → [(4-Fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride

HRID 1255034노트

반응식

HRID 1255034 반응식
C([O:3][C:4](=[O:21])[CH:5]([N:12]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)[CH3:13])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)C.O.[OH-].[Li+].[ClH:25]>C1COCC1.O>[ClH:25].[F:20][C:17]1[CH:18]=[CH:19][C:14]([N:12]([CH:5]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:4]([OH:21])=[O:3])[CH3:13])=[CH:15][CH:16]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 58556946Ethyl 2-((4-fluorophenyl)(methyl)amino)-2-phenylacetate

생성물 1

HCID 67124664[(4-Fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride수율 72%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of [(4-fluoro-phenyl)-methyl-amino]-phenyl-acetic acid ethyl ester (I70) (0.59 g, 2.05 mmol) in THF (10 mL) and water (10 mL), is added lithium hydroxide hydrate (0.26 g, 6.14 mmol). The reaction is stirred at RT for 3.5 hours and then at 70° C. for 24 hours. 3N HCl is added till pH is about 1 and the mixture is evaporated. Water (15 mL) is added and the residue is triturated obtaining a pale brown suspension that is filtered on a buckner funnel, washed with water and then with acetonitrile. The solid is dried under vacuum at 40° C. overnight to obtain intermediate I119 as a pale brown powder (0.44 g, 72% yield).

후처리

  1. waitat 70° C. for 24 hours
  2. customthe mixture is evaporated
  3. additionWater (15 mL) is added
  4. customthe residue is triturated
  5. customobtaining a pale brown suspension that
  6. filtrationis filtered on a buckner funnel
  7. washwashed with water
  8. customThe solid is dried under vacuum at 40° C. overnight

출처 및 근거

ORD 기록
ord-2bfda5f7273e4938a70ab43a8807bacd
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455646B2

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