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Thionyl Chloride → 5-Bromo-benzo[2,1,3]thiadiazole

HRID 335365
ノート
印刷プレビュー

反応式

HRID 335365 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[CH:6][CH:7]=1.CCN(C(C)C)C(C)C.O=[S:20](Cl)Cl>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[C:4]([CH:3]=1)=[N:9][S:20][N:8]=2
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 24386Thionyl ChlorideHCID 81531DiisopropylethylamineHCID 3235934-Bromobenzene-1,2-diamine

生成物 1

HCID 27762955-Bromo-benzo[2,1,3]thiadiazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-bromobenzene-1,2-diamine (5.236 g, 28.0 mmol) and Hunig's base (19.5 mL, 112 mmol) in dichloromethane (160 mL) was added SOCl2 (4.08 mL, 56 mmol) dropwise at room temperature. The resulting reaction mixture was heated to reflux overnight. The reaction mixture was then allowed to cool to room temperature, and quenched with 10% HCl until pH=2. The resulting mixture was extracted with dichloromethane (200 mL×4), dried over Na2SO4 and concentrated. The crude compound was purified by flash column chromatography (silica gel, chloroform) to afford 5-bromobenzo[1,2,5]thiadiazole as a brown solid which was used directly in the next step. 1H NMR (CDCl3 500 MHz): δ: 8.21 (d, 1H, J=1.5 Hz), 7.87 (d, 1H, J=8.5 Hz), 7.69 (dd, 1H, J=8.5, 1.5 Hz).

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux overnight
  4. customquenched with 10% HCl until pH=2
  5. extractionThe resulting mixture was extracted with dichloromethane (200 mL×4)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customThe crude compound was purified by flash column chromatography (silica gel, chloroform)

出典と根拠

ORDレコード
ord-1a6cb30ffed0483dbedae0a181a47844
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08883958B2

反応ノート

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