Boron trifluoride etherate → HCID 21449337, 화합물

HRID 597066노트

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HRID 597066 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 21449337HCID 21449337, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-584902398f454e8d96826209bbb86b6d
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012513

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