Hydrochloric Acid → HCID 69067890, 화합물

HRID 660891노트

반응식

HRID 660891 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([NH:9][CH2:10][C:11]([OH:13])=[O:12])[CH:6]=[CH:7][CH:8]=1.O1CCOCC1.[C:22](OC([O-])=O)([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23].Cl>C(=O)([O-])O.[Na+].C(#N)C>[C:25]([O:24][C:22]([N:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:14])([F:15])[F:1])[CH:4]=1)[CH2:10][C:11]([OH:13])=[O:12])=[O:23])([CH3:28])([CH3:27])[CH3:26]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 2478302-{[3-(trifluoromethyl)phenyl]amino}acetic acidHCID 22064466Tert-butyldicarbonate

생성물 1

HCID 69067890HCID 69067890, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 516892Sodium Bicarbonate용매

실험 절차

226 mg (1.03 mmol) of DL-[3-(trifluoromethyl)phenyl]-glycine are dissolved in 10 ml of an aqueous 5% sodium hydrogen carbonate solution and treated with 4 ml dioxan. 261 μl (1.13 mmol) of tert.-butyl dicarbonate are added and the mixture stirred overnight at RT. For the workup, the solution is carefully acidified to pH 2 with 1 N hydrochloric acid. The precipitated product is redissolved by addition of acetonitrile, and purified by preparative HPLC (Method 20). 135 mg (41% of theory) of the title compound are obtained.

후처리

  1. custompurified by preparative HPLC (Method 20)

출처 및 근거

ORD 기록
ord-e1bf9f93ece64672bfcd6b2581c71d22
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084481B2

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