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

HRID 1959064ノート

反応式

HRID 1959064 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-b54a011d57654e64b7e860dc26d5ee47
出典データセット
uspto-grants-2013_04
特許番号
US08410123B2

反応ノート

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