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Sulfuric Acid → 6-[(2-chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl) oxy]-alpha-methyl-1H-benzotriazol-1-acetaldehyde

HRID 963661
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HRID 963661 반응식
C[O:2][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>C(O)(=O)C.O.C(Cl)Cl>[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]=[O:2])[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

6

반응물 2

HCID 1118Sulfuric AcidHCID 867479446-[(2-chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl) oxy]-alpha-methyl-1H-benzotriazole-1-acetaldehyde dimethyl acetal

생성물 1

HCID 867479486-[(2-chloro-alpha,alpha,alpha,6-tetrafluoro-p-tolyl) oxy]-alpha-methyl-1H-benzotriazol-1-acetaldehyde

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매
HCID 6344Dichloromethane용매

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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 (20 g, 0.046 mole) in acetic acid is treated with 47 ml of 2.5N H2SO4, heated for 12 hours at 70° C., cooled and diluted with water and methylene chloride. The phases are separated and the aqueous phase is extracted with methylene chloride. The combined organic phases are dried (MgSO4), filtered through a pad of Al2O3, and concentrated in vacuo to afford the title compound as a solid, mp 107°-108° C., characterized by elemental and NMR analyses.

후처리

  1. temperaturecooled
  2. customThe phases are separated
  3. extractionthe aqueous phase is extracted with methylene chloride
  4. dry with materialThe combined organic phases are dried (MgSO4)
  5. filtrationfiltered through a pad of Al2O3
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-81dd2c0583f94e4a9383e6b857dd4013
출처 데이터셋
uspto-grants-1998_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05763615

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