Trifluoroacetic acid → HCID 67200202, 화합물

HRID 509974노트

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HRID 509974 반응식
C(OC(=O)[N:7]([C:18]1[N:23]=[CH:22][C:21]([CH:24]([C:26]2[C:34]3[C:29](=[N:30][CH:31]=[C:32]([O:35][CH3:36])[CH:33]=3)[N:28]([S:37]([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)(=[O:39])=[O:38])[CH:27]=2)O)=[CH:20][N:19]=1)[CH2:8][C:9]1[C:10]([O:16][CH3:17])=[N:11][CH:12]=[C:13]([F:15])[CH:14]=1)(C)(C)C.C([SiH](CC)CC)C.FC(F)(F)C(O)=O.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:40]1([S:37]([N:28]2[C:29]3=[N:30][CH:31]=[C:32]([O:35][CH3:36])[CH:33]=[C:34]3[C:26]([CH2:24][C:21]3[CH:22]=[N:23][C:18]([NH:7][CH2:8][C:9]4[C:10]([O:16][CH3:17])=[N:11][CH:12]=[C:13]([F:15])[CH:14]=4)=[N:19][CH:20]=3)=[CH:27]2)(=[O:39])=[O:38])[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=1

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 12052TriethylsilaneHCID 67201062HCID 67201062, 화합물

생성물 1

HCID 67200202HCID 67200202, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
80 °C

실험 절차

To {5-[(1-benzenesulfonyl-5-methoxy-1H-pyrrolo[2,3-b]pyridin-3-yl)-hydroxy-methyl]-pyrimidin-2-yl}-(5-fluoro-2-methoxy-pyridin-3-ylmethyl)-carbamic acid tert-butyl ester (124, 1 equivalent) in 10.0 mL of acetonitrile, triethylsilane (15.6 equivalents) and trifluoroacetic acid (16.9 equivalents) are added. The reaction is heated at 80° C. for 2 hours, then poured into aqueous potassium carbonate and extracted with ethyl acetate. The organic layer is dried over sodium sulfate, filtered and the filtrate concentrated under vacuum to provide the desired compound, which is used in the next step without further purification.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under vacuum

출처 및 근거

ORD 기록
ord-8581bd83d614468f8d989709420824f9
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096593B2

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