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

HRID 222282노트

반응식

HRID 222282 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-fa40a43cb5d14beea44c48174e127989
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08207186B2

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