Trifluoroacetic acid → HCID 22139438, 화합물

HRID 33802노트

반응식

HRID 33802 반응식
C(OC([N:8]1[C:21]2[CH:20]=[CH:19][CH:18]=[C:17]([C:22]3[O:23][C:24]([N:29]4[CH2:34][CH2:33][O:32][CH2:31][CH2:30]4)=[CH:25][C:26](=[O:28])[CH:27]=3)[C:16]=2[S:15][C:14]2[C:9]1=[CH:10][CH:11]=[CH:12][CH:13]=2)=O)(C)(C)C.FC(F)(F)C(O)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl>[N:29]1([C:24]2[O:23][C:22]([C:17]3[C:16]4[S:15][C:14]5[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=5)[NH:8][C:21]=4[CH:20]=[CH:19][CH:18]=3)=[CH:27][C:26](=[O:28])[CH:25]=2)[CH2:34][CH2:33][O:32][CH2:31][CH2:30]1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 235745714-(6-Morpholin-4-yl-4-oxo-4H-pyran-2-yl)-phenothiazine-10-carboxylic Acid tert-Butyl Ester

생성물 1

HCID 22139438HCID 22139438, 화합물수율 100.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of 4-(6-morpholin-4-yl-4-oxo-4H-pyran-2-yl)-phenothiazine-10-carboxylic acid tert-butyl ester (3.65 g, 7.63 mmol), in CH2Cl2 (30 ml) was added trifluoroacetic acid in a single portion. The mixture was stirred at room temperature for 20 hours whereupon the reaction was concentrated in vacuo to give a thick syrup that was basified in a dropwise fashion with saturated NaHCO3 (40 ml). The dark green mixture was then stirred at room temperature for 18 hours. The mixture was filtered and the filtrant retained, washed with water and dried to give the title compound as a dark green solid (2.89 g, 83.74% over 3 steps) m/z (LC-MS, ESP): 479 [M+H]+, RT=4.05 mins.

후처리

  1. concentrationwas concentrated in vacuo
  2. customto give a thick syrup that
  3. stirringThe dark green mixture was then stirred at room temperature for 18 hours
  4. filtrationThe mixture was filtered
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-5896ee51e23b424088bf49dff2cc197e
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429660B2

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