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Acetone → HCID 178466053, 화합물

HRID 2083233
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HRID 2083233 반응식
[OH:1][CH:2]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[O:10][CH:9]=[C:8]([C:14]1[NH:18][N:17]=[N:16][N:15]=1)[C:7]2=[O:19])[CH3:3].CC(C)=O.S(=O)(=O)(O)O>[O-2].[O-2].[O-2].[Cr+6].O>[C:2]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[O:10][CH:9]=[C:8]([C:14]1[NH:15][N:16]=[N:17][N:18]=1)[C:7]2=[O:19])(=[O:1])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 180AcetoneHCID 1118Sulfuric AcidHCID 178466054HCID 178466054, 화합물

생성물 1

HCID 178466053HCID 178466053, 화합물

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 962Water용매

실험 절차

To a solution of 2.58 parts of 6-(1-hydroxyethyl)-3-(1H-tetrazol-5-yl)chromone in 700 parts by volume of acetone kept at 9°-15° C there is added dropwise over a period of 30 minutes 4.5 parts by volume of a solution which is prepared from chromium trioxide, 97% sulfuric acid and water in a ratio of 6.0 parts: 3.6 parts by volume: 18 parts by volume. The reaction mixture is concentrated at a temperature lower than 30° C to a one-tenth volume and then admixed with 700 parts by volume of water to give precipitates. The precipitates are recovered by filtration and recrystallized from dimethylformamide. The procedure yields 1.70 parts of 6-acetyl-3-(1H-tetrazol-5-yl)chromone as colorless crystals.

후처리

  1. customkept at 9°-15° C
  2. additionthere is added dropwise over a period of 30 minutes 4.5 parts by volume of a solution which
  3. concentrationThe reaction mixture is concentrated at a temperature lower than 30° C to a one-tenth volume
  4. customto give
  5. customprecipitates
  6. filtrationThe precipitates are recovered by filtration
  7. customrecrystallized from dimethylformamide

출처 및 근거

ORD 기록
ord-66363c5f40db4d92ac69ac9e514df847
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04085116

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