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Sulfamide → HCID 53628413、化合物

HRID 2388882
ノート
印刷プレビュー

反応式

HRID 2388882 の反応式
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>[C:9]([O:8][C:7](=[O:13])[NH:6][CH:4]1[CH2:5][N:2]([S:30]([NH2:33])(=[O:32])=[O:31])[CH2:3]1)([CH3:10])([CH3:12])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 53628413HCID 53628413、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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 2 M 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.

後処理

  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 2 M 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

出典と根拠

ORDレコード
ord-aa6f5db5855045bba5e8ba730f031e53
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08269002B2

反応ノート

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