Phosphoric Acid → HCID 20145026, 화합물

HRID 1906017노트

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HRID 1906017 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14]([C:16]2[S:20][C:19]([NH:21]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)=[N:18][C:17]=2[CH3:41])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].OP(O)(O)=O>O>[NH2:21][C:19]1[S:20][C:16]([C:14]2[C:6]3[C:5](=[CH:4][C:3]([O:2][CH3:1])=[C:8]([O:9][CH3:10])[CH:7]=3)[CH2:11][CH2:12][N:13]=2)=[C:17]([CH3:41])[N:18]=1

참가 물질

4

반응물 2

HCID 1004Phosphoric AcidHCID 20144993HCID 20144993, 화합물

생성물 1

HCID 20145026HCID 20145026, 화합물수율 24.9%

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

A mixture of N-[2-(3,4-dimethoxyphenyl)ethyl]-4-methyl-2-tritylamino-5-thiazolecarboxamide (5.0 g) and polyphospholic acid (116% as H3PO4, 50 g) was stirred at 100° C. for 10 hours. After the reaction mixture was cooled, water (250 ml) was added and stirred for 1 hour. After removal of insoluble materials by filtration, the filtrate was neutralized with sodium carbonate. From the aqueous solution was extracted the desired compound with chloroform, and the extract was dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was triturated in diisopropyl ether to afford 1-(2-amino-4-methylthiazol-5-yl)-6,7-dimethoxy-3,4-dihydroisoquinoline (0.67 g).

후처리

  1. temperatureAfter the reaction mixture was cooled
  2. stirringstirred for 1 hour
  3. customAfter removal of insoluble materials
  4. filtrationby filtration
  5. extractionFrom the aqueous solution was extracted the desired compound with chloroform
  6. dry with materialthe extract was dried over magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe residue was triturated in diisopropyl ether

출처 및 근거

ORD 기록
ord-73cc14d2f4174adcaa1e35af2ba3d854
출처 데이터셋
uspto-grants-1987_03
특허 번호
US04649146

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