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Sulfamide → HCID 53628413, 화합물

HRID 1025009
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HRID 1025009 반응식
Cl.[NH:2]1[CH2:5][CH:4]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10])[CH2:3]1.CN(C1C2C(N(C)C)=CC=CC=2C=CC=1)C.[S:30](N)([NH2:33])(=[O:32])=[O:31]>O1CCOCC1>[NH2:33][S:30]([N:2]1[CH2:5][CH:4]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:10])([CH3:12])[CH3:11])[CH2:3]1)(=[O:32])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 82267SulfamideHCID 88675Proton spongeHCID 22101213tert-butyl N-(azetidin-3-yl)carbamate hydrochloride

생성물 1

HCID 53628413HCID 53628413, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of tert-butyl azetidin-3-ylcarbamate hydrochloride (prepared according to J. Antibiot. 1986, 39, 1243-1256, 0.755 g), Proton-Sponge® (0.85 g) and sulfamide (0.42 g) in dioxane (23 ml) was heated at reflux for 48 h. The residue was partitioned between H2O and EtOAc, and the aqueous layer then extracted with further EtOAc (×4). The combined organic extracts were washed quickly with 2M aqueous hydrochloric acid (×3) then with saturated aqueous sodium bicarbonate, H2O and saturated aqueous sodium chloride, dried with sodium sulfate, filtered and evaporated to afford the subtitle compound as a pale brown powder. Yield: 0.44 g

후처리

  1. temperatureat reflux for 48 h
  2. customThe residue was partitioned between H2O and EtOAc
  3. extractionthe aqueous layer then extracted with further EtOAc (×4)
  4. washThe combined organic extracts were washed quickly with 2M aqueous hydrochloric acid (×3)
  5. dry with materialwith saturated aqueous sodium bicarbonate, H2O and saturated aqueous sodium chloride, dried with sodium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-705ac7f0ffd44f87b2f684e4372d9cc1
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722883B2

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