Water → HCID 21631641, 화합물

HRID 383914노트

반응식

HRID 383914 반응식
[C:1]1([C:7]2[S:8][CH:9]=[CH:10][C:11]=2C(O)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1C=CC(P([N:29]=[N+]=[N-])(C2C=CC=CC=2)=O)=CC=1.C[C:33]([OH:36])(C)C.[OH2:37].[C:38]1([CH3:44])[CH:43]=CC=C[CH:39]=1>>[C:1]1([C:7]2[S:8][CH:9]=[CH:10][C:11]=2[NH:29][C:33](=[O:36])[O:37][C:38]([CH3:44])([CH3:43])[CH3:39])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 5

HCID 962WaterHCID 1140Toluene2회HCID 6386tert-ButanolHCID 199401P,P-Diphenylphosphinic azideHCID 8485112-phenyl-3-thiophenecarboxylic acid

생성물 1

HCID 21631641HCID 21631641, 화합물

실험 절차

To a solution of 2-phenylthiophene-3-carboxylic acid and TEA in toluene was added dropwise a solution of DPPA in toluene, followed by stirring at room temperature for 40 minutes, and then stirring at 90° C. for 60 minutes. To this solution was added tBuOH, followed by heating under reflux for 15 hours. To the reaction solution was added water, followed by extraction with EtOAc. The organic layer was washed with water and brine in this order, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by medium-pressure preparative liquid chromatography (silica gel, YAMAZEN YFLC WPrep2XY, hexane:EtOAc) to obtain tert-butyl (2-phenyl-3-thienyl)carbamate as a pale brown oil.

후처리

  1. stirringstirring at 90° C. for 60 minutes
  2. temperatureby heating
  3. temperatureunder reflux for 15 hours
  4. extractionfollowed by extraction with EtOAc
  5. washThe organic layer was washed with water and brine in this order
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by medium-pressure preparative liquid chromatography (silica gel, YAMAZEN YFLC WPrep2XY, hexane:EtOAc)

출처 및 근거

ORD 기록
ord-e71d5c8e44e241ce962a4d422586b6cf
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367696B2

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