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Hydrochloric Acid → 2-Chloro-6-cyclopropylimidazo[1,2-b]pyridazine-3-sulfonamide

HRID 969721
ノート
印刷プレビュー

反応式

HRID 969721 の反応式
[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][C:7]([CH:10]3[CH2:12][CH2:11]3)=[N:6][N:5]2[C:13]=1[S:14]([N:17]=CN(CC(C)C)CC(C)C)(=[O:16])=[O:15].Cl>O1CCOCC1>[Cl:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][C:7]([CH:10]3[CH2:12][CH2:11]3)=[N:6][N:5]2[C:13]=1[S:14]([NH2:17])(=[O:15])=[O:16]
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

4

反応物 2

HCID 313Hydrochloric AcidHCID 68535377HCID 68535377、化合物

生成物 1

HCID 230281432-Chloro-6-cyclopropylimidazo[1,2-b]pyridazine-3-sulfonamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

N′-(2-Chloro-6-cyclopropylimidazo[1,2-b]pyridazin-3-ylsulfonyl)-N,N-diisobutylformamidine (0.93 g, 2.26 mmol) was dissolved in dioxane (9.00 mL), and 36% concentrated hydrochloric acid (9.0 mL, 107 mmol) was added dropwise to the solution under stirring at 100° C. The mixture was stirred for 15 hours at 100 to 105° C., then left to cool to room temperature and concentrated under reduced pressure until crystals occurred. Water (30.0 mL) was poured into the residues, and the crystals were completely precipitated, then filtered, washed with water and washed with methanol, to give the title compound as white crystals. The yield was 0.31 g (50.4%).

後処理

  1. stirringThe mixture was stirred for 15 hours at 100 to 105° C.
  2. waitleft
  3. temperatureto cool to room temperature
  4. concentrationconcentrated under reduced pressure until crystals
  5. additionWater (30.0 mL) was poured into the residues
  6. customthe crystals were completely precipitated
  7. filtrationfiltered
  8. washwashed with water
  9. washwashed with methanol

出典と根拠

ORDレコード
ord-fb2def14be2c4402ad7a355c44504f60
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07307165B2

反応ノート

読み込み中…

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