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Hydrochloric Acid → HCID 15341023、化合物

HRID 612381
ノート
印刷プレビュー

反応式

HRID 612381 の反応式
[Cl:1][C:2]1[CH:23]=[C:22]([Cl:24])[CH:21]=[CH:20][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([S:16](Cl)(=[O:18])=[O:17])[CH:8]=[CH:9][C:10]=1[NH:11][S:12]([CH3:15])(=[O:14])=[O:13].Cl.[CH3:26][NH:27][CH3:28].[OH-].[Na+].Cl>O1CCOCC1>[CH3:26][N:27]([CH3:28])[S:16]([C:7]1[CH:8]=[CH:9][C:10]([NH:11][S:12]([CH3:15])(=[O:14])=[O:13])=[C:5]([O:4][C:3]2[CH:20]=[CH:21][C:22]([Cl:24])=[CH:23][C:2]=2[Cl:1])[CH:6]=1)(=[O:18])=[O:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10473Dimethylamine, hydrochlorideHCID 14798Sodium HydroxideHCID 23221647HCID 23221647、化合物

生成物 1

HCID 15341023HCID 15341023、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
0 °C

実験手順

3-(2,4-Dichlorophenoxy)-4-methylsulphonylaminobenzene-sulphonic acid chloride (1.12 g, 2.6 mmol) was dissolved in dioxan (5 ml) and at 0° C. added dropwise to a solution of dimethylamine hydrochloride (1.10 g, 13.4 mmol) in 1N aqueous NaOH (13 ml, 13 mmol) and dioxan (13 ml). The mixture was stirred for 1 hour at 0° C., acidified with 1N HCl and extracted with ethyl acetate. The combined organic phases were dried over MgSO4 and the solvent was evaporated off. The residue was purified by chromatography (silica gel, petroleum ether/ethyl acetate 6/4). Yield: 0.27 g=24% 13C (100 MHz, DMSO-d6) δ 150.02, 147.24, 133.01, 130.81, 130.42, 129.53, 129.18, 126.03, 123.74, 123.17, 122.57, 115.72, 41.03, 37.59

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe combined organic phases were dried over MgSO4
  3. customthe solvent was evaporated off
  4. customThe residue was purified by chromatography (silica gel, petroleum ether/ethyl acetate 6/4)

出典と根拠

ORDレコード
ord-579da13dec0149f1bab8b79ff659daad
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06004948

反応ノート

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