Boron trifluoride etherate → HCID 21449337、化合物

HRID 597066

反応式

HRID 597066 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([N:12]3[C:20]4[C:15](=[CH:16][C:17]([O:21][CH3:22])=[CH:18][CH:19]=4)[C:14]([CH2:23][C:24]([OH:26])=[O:25])=[C:13]3[CH3:27])=[N:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.B(F)(F)F.[CH3:32]COCC.C([O-])(=O)C.[Na+]>CO>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([N:12]3[C:20]4[C:15](=[CH:16][C:17]([O:21][CH3:22])=[CH:18][CH:19]=4)[C:14]([CH2:23][C:24]([O:26][CH3:32])=[O:25])=[C:13]3[CH3:27])=[N:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8000Boron trifluoride etherateHCID 517045Sodium AcetateHCID 101940031-(7-Chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetic acid

生成物 1

HCID 21449337HCID 21449337、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-(7-chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetic acid (1.0g.) in dry methanol (50ml.) was added freshly distilled boron trifluoride etherate (0.5ml.), and the dark red solution was heated under reflux for 30 mins. To the solution was added saturated sodium acetate solution (5ml.), and the mixture was concentrated in vacuo. The residual mixture was shaken with a mixture of water (50ml.) and chloroform (30ml.). The aqueous layer was separated and extracted with further chloroform (2 × 20 ml.), and the combined extracts were washed successively with saturated sodium hydrogen carbonate solution (2 × 20ml.), water (10ml.) and saturated sodium chloride solution (15ml.). After drying, the extracts were evaporated to give methyl 1(7-chloroquinazolin-4-yl)-5-methoxy-2-methylindol-3-ylacetate, m.p. 111°-113° C.

後処理

  1. temperaturethe dark red solution was heated
  2. temperatureunder reflux for 30 mins
  3. concentrationthe mixture was concentrated in vacuo
  4. customThe aqueous layer was separated
  5. extractionextracted with further chloroform (2 × 20 ml.)
  6. washthe combined extracts were washed successively with saturated sodium hydrogen carbonate solution (2 × 20ml.), water (10ml.) and saturated sodium chloride solution (15ml.)
  7. customAfter drying
  8. customthe extracts were evaporated

出典と根拠

ORDレコード
ord-584902398f454e8d96826209bbb86b6d
出典データセット
uspto-grants-1977_03
特許番号
US04012513

関連ノート

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