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

HRID 969721
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HRID 969721 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68535377HCID 68535377, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-fb2def14be2c4402ad7a355c44504f60
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07307165B2

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