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Sulfuric Acid → 6-[(2-Chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl)oxy]-alpha-methyl-1h-benzotriazole-1-acetaldehyde oxime

HRID 1110004
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인쇄 미리보기

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HRID 1110004 반응식
CO[CH:3](OC)[CH:4]([CH3:27])[N:5]1[C:9]2[CH:10]=[C:11]([O:14][C:15]3[CH:20]=[C:19]([F:21])[C:18]([C:22]([F:25])([F:24])[F:23])=[C:17]([Cl:26])[CH:16]=3)[CH:12]=[CH:13][C:8]=2[N:7]=[N:6]1.OS(O)(=O)=O.Cl.[NH2:36][OH:37]>C(O)(=O)C.O.N1C=CC=CC=1.C(O)C>[Cl:26][C:17]1[CH:16]=[C:15]([O:14][C:11]2[CH:12]=[CH:13][C:8]3[N:7]=[N:6][N:5]([CH:4]([CH3:27])[CH:3]=[N:36][OH:37])[C:9]=3[CH:10]=2)[CH:20]=[C:19]([F:21])[C:18]=1[C:22]([F:25])([F:24])[F:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 1118Sulfuric AcidHCID 443297Hydroxyamine hydrochlorideHCID 86747944HCID 86747944, 화합물

생성물 1

HCID 867479466-[(2-Chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl)oxy]-alpha-methyl-1h-benzotriazole-1-acetaldehyde oxime

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 702
Ethanol
용매
HCID 962Water용매
HCID 1049Pyridine용매

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온도
70 °C

실험 절차

A solution of 6-[(2-chloro-α,α,α,6-tetrafluoro-p-tolyl)oxy]-α-methyl-1H-benzotriazole-1-acetaldehyde dimethyl acetal (23.0 g, 0.053 mole) in acetic acid is treated with 54 ml of 2.5N H2SO4 and stirred at 70° C. for 12 hours. A 15 ml portion of the reaction solution is diluted to a total volume of 100 ml with water, the resulting precipitate is separated, washed with water, treated with a solution of hydroxylamine hydrochloride (1.0 g, 0.014 mole) in pyridine and ethanol, heated at 85° C. for several hours, cooled and concentrated in vacuo to give a solid residue. Recrystallization from aqueous ethanol, ethanol and toluene gives the title compound mp 148°-151° C., identified by elemental and NMR analyses.

후처리

  1. customthe resulting precipitate is separated
  2. washwashed with water
  3. temperatureheated at 85° C. for several hours
  4. temperaturecooled
  5. concentrationconcentrated in vacuo
  6. customto give a solid residue
  7. customRecrystallization from aqueous ethanol, ethanol and toluene

출처 및 근거

ORD 기록
ord-c0157d7c0bd84d1daaf999cc48cf68ee
출처 데이터셋
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05324711

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