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Ethanol → 2,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine

HRID 65675
노트
인쇄 미리보기

반응식

HRID 65675 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]=[C:10]2[C:15](=O)[C:14](=[CH:17][C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[C:20]([CH3:26])[C:19]=3[CH3:27])[CH2:13][O:12][CH2:11]2)=[C:5]([CH3:28])[C:4]=1[CH3:29].[NH2:30][C:31]1[S:32][CH2:33][CH2:34][N:35]=1.CCO>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[N:35]3[CH2:34][CH2:33][S:32][C:31]3=[N:30][C:15]3[C:14](=[CH:17][C:18]4[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[C:20]([CH3:26])[C:19]=4[CH3:27])[CH2:13][O:12][CH2:11][C:10]2=3)=[C:5]([CH3:28])[C:4]=1[CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 156894,5-Dihydro-2-thiazolamineHCID 54006504Tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one

생성물 1

HCID 217866812,3,8,9-Tetrahydro-5-(4-methoxy-2,3-dimethylphenyl)-9-[(4-methoxy-2,3-dimethylphenyl)-methylene]-5H,6H-pyrano[4,3-d]thiazolo[3,2-a]pyrimidine수율 74.5%

시약·촉매·용매 1

HCID 6212
Chloroform
용매

실험 절차

A stirred solution of tetrahydro-3,5-bis[(4-methoxy-2,3-dimethylphenyl)methylene]-4H-pyran-4-one (3.0 g, 7.6 mmole) and 2-amino-2-thiazoline (1.0 g, 9.7 mmole) in 75 ml of CHCl3 is heated at reflux temperature for 72 hours. After cooling, the solution is filtered to remove a small amount of insoluble material. The solvent is evaporated to give an oily residue. Trituration with warm EtOH yields 2.7 g of a yellow solid, m.p. 226°-228° d. Crystallization from 15 ml of DMF gives 2.3 g (63%) of cream colored product, m.p. 235°-237°.

후처리

  1. temperatureat reflux temperature for 72 hours
  2. temperatureAfter cooling
  3. filtrationthe solution is filtered
  4. customto remove a small amount of insoluble material
  5. customThe solvent is evaporated
  6. customto give an oily residue

출처 및 근거

ORD 기록
ord-0216767bb51d4822929f14d5e9fea3a9
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04128648

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