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Triethylamine → 2,6-Dichloro-3-(propylsulfonamido)benzoic acid

HRID 1943858
ノート
印刷プレビュー

反応式

HRID 1943858 の反応式
[NH2:1][C:2]1[C:3]([Cl:12])=[C:4]([C:8]([Cl:11])=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].C(N(CC)CC)C.[CH2:20]([S:23](Cl)(=[O:25])=[O:24])[CH2:21][CH3:22]>ClCCl>[Cl:12][C:3]1[C:2]([NH:1][S:23]([CH2:20][CH2:21][CH3:22])(=[O:25])=[O:24])=[CH:10][CH:9]=[C:8]([Cl:11])[C:4]=1[C:5]([OH:7])=[O:6]
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

5

反応物 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 5213073-Amino-2,6-dichlorobenzoic acid

生成物 1

HCID 580953672,6-Dichloro-3-(propylsulfonamido)benzoic acid収率 74.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

3-Amino-2,6-dichlorobenzoic acid (1.40 g, 6.82 mmol) was dissolved in dry dichloromethane (66.7 mL). Triethylamine (4.09 mL, 29.4 mmol) was added, and the mixture was chilled to 0° C. Propane-1-sulfonyl chloride (2.48 mL, 22 mmol) was then added via syringe. Once the addition was complete, the mixture was allowed to warm to ambient temperature and stir for 1 hour. The mixture was concentrated in vacuo and diluted with diethyl ether. The mixture was washed with 0.25M NaOH (80 mL), and the aqueous layer was acidified to a pH of 1 using 1.0M HCl. The aqueous layer was extracted with 15% 2-propanol:DCM (2×300 mL). The organic layer was collected, dried over sodium sulfate, and concentrated to afford 2,6-dichloro-3-(propylsulfonamido)benzoic acid (1.55 g, 4.96 mmol, 74.4% yield). 1H NMR (400 MHz, d6-DMSO) δ 9.77-9.75 (s, 1H), 7.84-7.80 (d, 1H), 7.71-7.68 (d, 1H), 3.82-3.72 (m, 2H), 1.89-1.70 (m, 2H), 1.05-1.03 (m, 3H).

後処理

  1. additionOnce the addition
  2. temperatureto warm to ambient temperature
  3. concentrationThe mixture was concentrated in vacuo
  4. additiondiluted with diethyl ether
  5. washThe mixture was washed with 0.25M NaOH (80 mL)
  6. extractionThe aqueous layer was extracted with 15% 2-propanol
  7. customThe organic layer was collected
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-9417a995f45c4805b138d4f52991ea3a
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08394795B2

反応ノート

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