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Thiophene → HCID 23339052, 화합물

HRID 236757
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인쇄 미리보기

반응식

HRID 236757 반응식
S1C=CC=C1.[C:6]1(=O)[CH2:10][CH2:9][CH2:8][CH2:7]1.[NH:12]1[CH2:17][CH2:16][CH:15]([NH:18][C:19]2[N:24]=[CH:23][CH:22]=[CH:21][N:20]=2)[CH2:14][CH2:13]1.[H][H]>[Pd].CO.C(O)C>[CH:6]1([N:12]2[CH2:13][CH2:14][CH:15]([NH:18][C:19]3[N:20]=[CH:21][CH:22]=[CH:23][N:24]=3)[CH2:16][CH2:17]2)[CH2:10][CH2:9][CH2:8][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8030ThiopheneHCID 8452CyclopentanoneHCID 18374737N-(Piperidin-4-yl)pyrimidin-2-amineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 23339052HCID 23339052, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매
HCID 702
Ethanol
용매
HCID 887Methanol용매

실험 절차

To 0.5 parts of a solution of 2 parts of thiophene in 40 parts of ethanol, are added 2 parts of cyclopentanone, 5.5 parts of N-(4-piperidinyl)-2-pyrimidinamine and 120 parts of methanol. The whole is hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. The residue is taken up in 4-methyl-2-pentanone and a small amount of trichloromethane. The whole is washed twice with a diluted sodium hydroxide solution, dried, filtered and evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 2.3 parts of N-(1-cyclopentyl-4-piperidinyl)-2-pyrimidinamine; mp. 118° C.

후처리

  1. filtrationthe catalyst is filtered off
  2. customthe filtrate is evaporated
  3. washThe whole is washed twice with a diluted sodium hydroxide solution
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is crystallized from 2,2'-oxybispropane
  8. filtrationThe product is filtered off
  9. customdried

출처 및 근거

ORD 기록
ord-50496a18ee934b539da1a1c1aa640892
출처 데이터셋
uspto-grants-1979_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04157393

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