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ethyl 3-oxotetrahydro-2H-thiopyran-2-carboxylate → HCID 178515237, 화합물

HRID 973541
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HRID 973541 반응식
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([N:7]2[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[N:3]=1.O=[C:14]1[CH2:19][CH2:18][CH2:17][S:16][CH:15]1[C:20](OCC)=[O:21]>C(O)(=O)C.O>[N:7]1([C:4]2[N:3]=[C:2]3[NH:1][C:14]4[CH2:19][CH2:18][CH2:17][S:16][C:15]=4[C:20](=[O:21])[N:6]3[N:5]=2)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1
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참가 물질

5

반응물 2

HCID 12269128ethyl 3-oxotetrahydro-2H-thiopyran-2-carboxylateHCID 137896925-(1-Piperidinyl)-1H-1,2,4-triazol-3-amine

생성물 1

HCID 178515237HCID 178515237, 화합물수율 82.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

16.7 g (0.1 mole) of 5-amino-3-piperidino-1H-1,2,4-triazole are dissolved in 10 ml of acetic acid and 18.8 g (0.1 mole) of ethyl 3-oxo-3,4,5,6-tetrahydro-2H-thiopyrane-2-carboxylate are added, then the reaction mixture is boiled for 10 minutes. The thick crystal mass thus obtained is diluted with 100 ml of water, the precipitated product is filtered off, washed with i-propanol and recrystallized from dimethylformamide. Thus 23.3 g (82.2%) of 2-piperidino-5,7,8,9-tetrahydrothiopyrano[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidine-5(10H)-one are obtained with a melting point above 350° C.

후처리

  1. customThe thick crystal mass thus obtained
  2. filtrationthe precipitated product is filtered off
  3. washwashed with i-propanol
  4. customrecrystallized from dimethylformamide

출처 및 근거

ORD 기록
ord-38788ccf1ae143fa908e9ff8cad4b8fa
출처 데이터셋
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05064826

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