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Phosphorus oxybromide → HCID 86687897, 화합물

HRID 868982
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HRID 868982 반응식
[CH3:1][C:2]1[N:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](=O)[NH:7]2.P(Br)(Br)([Br:16])=O.C(=O)(O)[O-].[Na+]>>[Br:16][C:6]1[CH:5]=[CH:4][C:3]2[C:8](=[C:9]([CH3:12])[CH:10]=[N:11][C:2]=2[CH3:1])[N:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 24613Phosphorus oxybromideHCID 516892Sodium BicarbonateHCID 701163661,6-Naphthyridin-2(1H)-one, 5,8-dimethyl-

생성물 1

HCID 86687897HCID 86687897, 화합물수율 22.1%

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온도
110 °C

실험 절차

A mixture of 5,8-dimethyl-1,6-naphthyridin-2(1H)-one (2.1 g, 12 mmol) and phosphoryl tribromide (5 g) was heated to 110° C. for 1 h, cooled, diluted with ice water, and neutralized with saturated sodium bicarbonate solution. The aqueous phase was extracted with DCM (100 mL×3), and the combined organic layers were dried with sodium sulfate and purified by column chromatography to give 0.63 g of the product as a pale white solid. MS (ESI): m/z 237.0 [M+H]+.

후처리

  1. temperaturecooled
  2. extractionThe aqueous phase was extracted with DCM (100 mL×3)
  3. dry with materialthe combined organic layers were dried with sodium sulfate
  4. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-f5fb156861a14d9cb5cf1a84f223b40e
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969349B2

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