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Dichloromethane → HCID 67345859, 화합물

HRID 1669400
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HRID 1669400 반응식
[S:1](N)([NH2:4])(=[O:3])=[O:2].[CH:6]1([CH2:9][NH:10][CH2:11][CH:12]([O:15][CH3:16])[O:13][CH3:14])[CH2:8][CH2:7]1.C(Cl)Cl>O1CCOCC1>[CH:6]1([CH2:9][N:10]([CH2:11][CH:12]([O:13][CH3:14])[O:15][CH3:16])[S:1]([NH2:4])(=[O:3])=[O:2])[CH2:7][CH2:8]1
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참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 82267SulfamideHCID 45792518(cyclopropylmethyl)(2,2-dimethoxyethyl)amine

생성물 1

HCID 67345859HCID 67345859, 화합물수율 68%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Sulfamide (5 eq) was added to a solution of N-(cyclopropylmethyl)-(2,2-dimethoxyethanamine) in dioxane (0.12 M). The reaction was stirred at reflux overnight. The solvent was removed in vacuo, the residue taken up in EtOAc and washed with H2O, brine, before being dried (Na2SO4), filtered and concentrated in vacuo to give the crude material. DCM was added and the resultant precipitate removed by filtration, while the filtrate was concentrated in vacuo to afford the product (68%). 1H NMR (300 MHz, DMSO-d6, 300 K) δ 0.15-0.19 (m, 2H), 0.44-0.47 (m, 2H), 1.03-1.05 (m, 1H), 2.95-2.98 (m, 2H), 3.17-3.19 (m, 2H), 3.28 (s, 6H), 4.51 (t, J 5.0, 1H), 6.63 (s, 2H).

후처리

  1. temperatureat reflux overnight
  2. customThe solvent was removed in vacuo
  3. washwashed with H2O, brine
  4. dry with materialbefore being dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto give the crude material
  8. customthe resultant precipitate removed by filtration, while the filtrate
  9. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-16e70f4f07b14205afdef4fd1c776548
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989438B2

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