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

HRID 1025005ノート

反応式

HRID 1025005 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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: 51 mg

後処理

  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

出典と根拠

ORDレコード
ord-7b5ba17e810044c18813b7c4d14862f5
出典データセット
uspto-grants-2014_05
特許番号
US08722883B2

反応ノート

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