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Water → HCID 23366165, 화합물

HRID 1080886
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HRID 1080886 반응식
[Cl:1][C:2]1[C:11]([Cl:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:13](Cl)=[O:14])[CH:8]=2)[N:3]=1.[BH4-].[Na+].O>O1CCOCC1>[Cl:1][C:2]1[C:11]([Cl:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH2:13][OH:14])[CH:8]=2)[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 747146-Quinoxalinecarbonyl chloride, 2,3-dichloro-HCID 4311764Sodium borohydride

생성물 1

HCID 23366165HCID 23366165, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a suspension of 25.3 g portion of 2,3-dichloroquinoxaline-6-carbonyl chloride synthesized in accordance with the procedure disclosed in JP-A 57-98274 in 400 ml of anhydrous 1,4-dioxane, was added 14.0 g of sodium borohydride, and the mixture was stirred at room temperature for 10 minutes in an atmosphere of nitrogen. With cooling on an ice bath, to this was added dropwise 100 ml of water. Thereafter, 1,4-dioxane was evaporated under a reduced pressure, and the resulting residue was purified by chromatography on a silica gel column (eluent, hexane/ethyl acetate) to obtain 8.75 g of 2,3-dichloro-6-hydroxymethylquinoxaline.

후처리

  1. customsynthesized in accordance with the procedure
  2. temperatureWith cooling on an ice bath
  3. customThereafter, 1,4-dioxane was evaporated under a reduced pressure
  4. customthe resulting residue was purified by chromatography on a silica gel column (eluent, hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-2d182e9289154a7cb188372a3fe947cd
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05583227

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