Water → ((2-Thienylcarbonyl)amino)acetic acid

HRID 1178074

반응식

HRID 1178074 반응식
O[Li].O.C([O:6][C:7](=[O:17])[CH2:8][NH:9][C:10]([C:12]1[S:13][CH:14]=[CH:15][CH:16]=1)=[O:11])C.C1COCC1.O>CO>[S:13]1[CH:14]=[CH:15][CH:16]=[C:12]1[C:10]([NH:9][CH2:8][C:7]([OH:17])=[O:6])=[O:11]

참가 물질

6

반응물 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 168937Lithium hydroxide, monohydrateHCID 1720748Ethyl N-(thiophene-2-carbonyl)glycinate

생성물 1

HCID 679227((2-Thienylcarbonyl)amino)acetic acid수율 70%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

LiOH.H2O (110 mg, 2.63 mmol) was added to a solution of [(thiophene-2-carbonyl)-amino]-acetic acid ethyl ester (140 mg, 0.66 mmol) in a mixture of MeOH (5 mL), THF (2.5 mL) and H2O (2.5 mL). The resulting mixture was stirred for 3 hrs at room temperature. The MeOH and THF were evaporated and the resulting residue was diluted with water (2 mL), acidified with citric acid and extracted with EtOAc. The organic layer was washed with brine solution, dried over Na2SO4 and concentrated under reduced pressure to afford [(thiophene-2-carbonyl)-amino]-acetic acid in 70% yield. LC-MS purity: 92%.

후처리

  1. customThe MeOH and THF were evaporated
  2. additionthe resulting residue was diluted with water (2 mL)
  3. extractionextracted with EtOAc
  4. washThe organic layer was washed with brine solution
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-019afa39c9b64df397d52169620cad22
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07842696B2

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