Hydrochloric Acid → HCID 21867424、化合物

HRID 857395

反応式

HRID 857395 の反応式
[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([C:12](OC)=[O:13])[NH:6]2.[H-].C([Al+]CC(C)C)C(C)C.Cl>C1COCC1>[Br:1][C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH2:12][OH:13])[NH:6]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21225700DiisobutylaluminumhydrideHCID 21867463Methyl 4-bromo-6-fluoro-1H-indole-2-carboxylate

生成物 1

HCID 21867424HCID 21867424、化合物収率 96.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-30 °C

実験手順

To a solution of methyl 4-bromo-6-fluoro-1H-indole-2-carboxylate (3 g, 11 mmol) in THF (50 mL) at −30° C. was added diisobutylaluminum hydride (33 mmol, 1.5M toluene solution). The mixture was stirred for 1 hour at −30° C. and 1N HCl was added. The phases were separated and the aqueous layer was extracted with Et2O. The combined organic layers were dried over Na2SO4 and concentrated to give 2.6 g of the title compound used as such.

後処理

  1. customThe phases were separated
  2. extractionthe aqueous layer was extracted with Et2O
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-62c19ebd538d4c77bd4a41527a3c3744
出典データセット
uspto-grants-2006_12
特許番号
US07144913B2

関連ノート

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