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Ethanol → 2-Imino-5-[4-[2-(5-methyl-2-phenyl-oxazole-4-yl)-ethoxy]-benzothiophene-7-yl]-methyl-thiazolidine-4-one

HRID 1596798
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HRID 1596798 반응식
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][CH2:14][O:15][C:16]1[C:21]2[CH:22]=[CH:23][S:24][C:20]=2[C:19](N)=[CH:18][CH:17]=1.[NH2:26][C:27]([NH2:29])=[S:28].[C:30]([O-:33])(=O)[CH3:31].[Na+].[CH2:35](O)C>>[NH:26]=[C:27]1[N:29]([CH3:35])[C:30](=[O:33])[CH:31]([C:19]2[C:20]3[S:24][CH:23]=[CH:22][C:21]=3[C:16]([O:15][CH2:14][CH2:13][C:3]3[N:4]=[C:5]([C:7]4[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=4)[O:6][C:2]=3[CH3:1])=[CH:17][CH:18]=2)[S:28]1
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참가 물질

5

반응물 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 2723790ThioureaHCID 154856655-Methyl-4-[2-(7-amino-benzothiophene-4-yloxy)-ethyl]-2-phenyl-oxazole

생성물 1

HCID 184022522-Imino-5-[4-[2-(5-methyl-2-phenyl-oxazole-4-yl)-ethoxy]-benzothiophene-7-yl]-methyl-thiazolidine-4-one

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온도
2 °C

실험 절차

190 g (0.380 mol) of 5-methyl-4-[2-(7-amino-benzothiophene-4-yloxy)-ethyl]-2-phenyl-oxazole were suspended in 2.85 1 of ethanol. 31.6 g (0.415 mol) of thiourea and 34.8 g of sodium acetate were added. After boiling for about 18 hours (reflux) the reaction mixture was cooled to 0 to 4° C. and stirred for 1.5 hours at this temperature. The precipitate was filtered with suction and washed twice with 250 mnl cold ethanol. 1.91 of water was added to the residue, the mixture was stirred for 10 minutes and the precipitate was filtered with suction and dried for 24 hours at 80° C. (vacuum).

후처리

  1. temperature(reflux) the reaction mixture
  2. filtrationThe precipitate was filtered with suction
  3. washwashed twice with 250 mnl cold ethanol
  4. addition1.91 of water was added to the residue
  5. stirringthe mixture was stirred for 10 minutes
  6. filtrationthe precipitate was filtered with suction
  7. customdried for 24 hours at 80° C. (vacuum)

출처 및 근거

ORD 기록
ord-4338e03645c048cc864b9c1b7be042f3
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06291685B1

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