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Hydrochloric Acid → HCID 14722565, 화합물

HRID 1073182
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HRID 1073182 반응식
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[C:11]([Cl:12])=[CH:10][C:9]([C:13]#[N:14])=[CH:8][C:7]=1[Cl:15])=[O:4].CC(O)C.Cl.[H][H]>[Pd].CO>[NH2:14][CH2:13][C:9]1[CH:8]=[C:7]([Cl:15])[C:6]([NH:5][C:3](=[O:4])[CH2:2][Cl:1])=[C:11]([Cl:12])[CH:10]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 147225642-chloro-N-(2,6-dichloro-4-cyanophenyl)acetamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 14722565HCID 14722565, 화합물수율 100%

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 887
Methanol
용매

실험 절차

A mixture of 10.5 parts of 2-chloro-N-(2,6-dichloro-4-cyanophenyl) acetamide, 22 parts of 2-propanol, saturated with hydrogen chloride and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was taken up in water and treated with a sodium hydroxide solution 50%. The product was extracted twice with dichloromethane. The combined extracts were dried, filtered and evaporated, yielding 10.7 parts (100%) of N-[4-(aminomethyl)-2,6-dichlorophenyl]-2-chloroacetamide as a residue (int. 100).

후처리

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. additiontreated with a sodium hydroxide solution 50%
  4. extractionThe product was extracted twice with dichloromethane
  5. customThe combined extracts were dried
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-7a7dea698e594c72b8641bbaa229bd6d
출처 데이터셋
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04968684

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