Tert-butyl {[methyl(tetrahydrofuran-3-yl)amino]sulfonyl}carbamate → N-methyl-N-(tetrahydrofuran-3-yl)sulfamide

HRID 222282ノート

反応式

HRID 222282 の反応式
[CH3:1][N:2]([CH:14]1[CH2:18][CH2:17][O:16][CH2:15]1)[S:3]([NH:6]C(=O)OC(C)(C)C)(=[O:5])=[O:4]>C(Cl)Cl.FC(F)(F)C(O)=O>[CH3:1][N:2]([CH:14]1[CH2:18][CH2:17][O:16][CH2:15]1)[S:3]([NH2:6])(=[O:5])=[O:4]

参加物

4

反応物 1

HCID 86609783Tert-butyl {[methyl(tetrahydrofuran-3-yl)amino]sulfonyl}carbamate

生成物 1

HCID 67364770N-methyl-N-(tetrahydrofuran-3-yl)sulfamide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

tert-butyl {[methyl(tetrahydrofuran-3-yl)amino]sulfonyl}carbamate (1.47 g, 5.23 mmol) was dissolved in 70 mL of CH2Cl2 and 45 mL of trifluoroacetic acid. After 1 h the solution was concentrated in vacuo, diluted in CH2Cl2, washed with saturated aqueous NaHCO3 and brine, then dried over Na2SO4. The solution was concentrated in vacuo to afford the title compound. 1H NMR (600 MHz, DMSO-d6) δ 4.25-4.31 (m, 1H); 3.79-3.84 (m, 1H); 3.58-3.66 (m, 2H); 3.47-3.52 (m, 1H); 2.56 (s, 3H), 2.04-2.10 (m, 1H); 1.81-1.88 (m, 1H).

後処理

  1. concentrationAfter 1 h the solution was concentrated in vacuo
  2. additiondiluted in CH2Cl2
  3. washwashed with saturated aqueous NaHCO3 and brine
  4. dry with materialdried over Na2SO4
  5. concentrationThe solution was concentrated in vacuo

出典と根拠

ORDレコード
ord-fa40a43cb5d14beea44c48174e127989
出典データセット
uspto-grants-2012_06
特許番号
US08207186B2

反応ノート

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