Trifluoroacetic acid → N-{2-[(2,3-Difluorobenzyl)thio]-6-methoxypyrimidin-4-yl}-1,4-diazepane-1-sulfonamide

HRID 1175514노트

반응식

HRID 1175514 반응식
[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:22][CH2:21][CH2:20][N:19](C(OC(C)(C)C)=O)[CH2:18][CH2:17]2)(=[O:15])=[O:14])[CH:9]=[C:8]([O:30][CH3:31])[N:7]=1.C(O)(C(F)(F)F)=O>CO>[F:1][C:2]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:3]=1[CH2:4][S:5][C:6]1[N:11]=[C:10]([NH:12][S:13]([N:16]2[CH2:22][CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)(=[O:14])=[O:15])[CH:9]=[C:8]([O:30][CH3:31])[N:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 53628411tert-Butyl 4-[({2-[(2,3-difluorobenzyl)thio]-6-methoxypyrimidin-4-yl}amino)sulfonyl]-1,4-diazepane-1-carboxylate

생성물 1

HCID 59558769N-{2-[(2,3-Difluorobenzyl)thio]-6-methoxypyrimidin-4-yl}-1,4-diazepane-1-sulfonamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of tert-Butyl 4-[({2-[(2,3-difluorobenzyl)thio]-6-methoxypyrimidin-4-yl}amino)sulfonyl]-1,4-diazepane-1-carboxylate (the product of step i, 0.22 g) in 1:1 TFA:methanol (6 ml) was stirred at room temperature for 3 h then the volatiles evaporated and 7M ammonia in methanol (5 ml) added to the residue. The solution was stirred for 30 min then the volatiles evaporated and the resulting solid washed with methanol, DCM, dimethyl sulfoxide and H2O to afford the title compound as a white powder. Yield: δ 1 mg

후처리

  1. customthe volatiles evaporated
  2. addition7M ammonia in methanol (5 ml) added to the residue
  3. customthe volatiles evaporated
  4. washthe resulting solid washed with methanol, DCM, dimethyl sulfoxide and H2O

출처 및 근거

ORD 기록
ord-3110567cc20d4adcac7aeabbab741f28
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838675B2

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