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1,1-Dimethylhydrazine → HCID 13849570、化合物

HRID 2413517
ノート
印刷プレビュー

反応式

HRID 2413517 の反応式
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11](Cl)(=[O:13])=[O:12])(=[O:4])=[O:3].[CH3:15][N:16]([CH3:18])[NH2:17]>O1CCCC1>[CH3:15][N:16]([CH3:18])[NH:17][S:11]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[S:2]([NH2:1])(=[O:4])=[O:3])(=[O:13])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 59761,1-DimethylhydrazineHCID 138495692-Sulfamoylbenzene-1-sulfonyl chloride

生成物 1

HCID 13849570HCID 13849570、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 1.28 g of 2-(aminosulfonyl)benzenesulfonyl chloride in 12 mL of dry tetrahydrofuran (THF) was cooled to -65° C. and a solution of 0.88 mL of 1,1-dimethylhydrazine in 12 mL of dry THF added dropwise. The resulting mixture was allowed to warm to room temperature, filtered, and the filtrate concentrated in vacuo. The solid residue was partitioned between water and ethyl acetate, the organic phase was separated, washed with water, washed with brine, dried (MgSO4), concentrated in vacuo, and the residue triturated with 1-chlorobutane to provide 1.07 g of the subject compound, m.p. 122°-124° C. (dec).

後処理

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated in vacuo
  3. customThe solid residue was partitioned between water and ethyl acetate
  4. customthe organic phase was separated
  5. washwashed with water
  6. washwashed with brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo
  9. customthe residue triturated with 1-chlorobutane

出典と根拠

ORDレコード
ord-b051e3627c944d079077d038f15ce969
出典データセット
uspto-grants-1988_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04718938

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート