Hydrochloric Acid → 6-Bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazole

HRID 41267

反応式

HRID 41267 の反応式
[Br:1][C:2]1[C:22](C(O)=O)=[C:5]2[S:6][CH:7]=[C:8]([C:9]3[C:14]([O:15][CH3:16])=[CH:13][C:12]([CH2:17][O:18][CH3:19])=[CH:11][C:10]=3[O:20][CH3:21])[N:4]2[N:3]=1.Cl>O1CCOCC1>[Br:1][C:2]1[CH:22]=[C:5]2[S:6][CH:7]=[C:8]([C:9]3[C:10]([O:20][CH3:21])=[CH:11][C:12]([CH2:17][O:18][CH3:19])=[CH:13][C:14]=3[O:15][CH3:16])[N:4]2[N:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58223485HCID 58223485、化合物

生成物 1

HCID 582234186-Bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazole収率 25%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a 1,4-dioxane (90.0 mL) solution of 6-bromo-3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]pyrazolo[5,1-b][1,3]thiazole-7-carboxylic acid (5.00 g, 11.7 mmol) was added concentrated hydrochloric acid (14.9 mL) and the mixture was heated to reflux for 13 hours. After the reaction was completed, the solvent was distilled off under reduced pressure, water (50 mL) was added to the residue, and the precipitated solid was subjected to suction filtration and dried to obtain the title compound (1.12 g, 2.92 mmol).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 13 hours
  3. distillationthe solvent was distilled off under reduced pressure, water (50 mL)
  4. additionwas added to the residue
  5. filtrationthe precipitated solid was subjected to suction filtration
  6. customdried

出典と根拠

ORDレコード
ord-7e5e6bca274745aa8f6228e6e192d79a
出典データセット
uspto-grants-2013_09
特許番号
US08530504B2

関連ノート

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