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Ethanol → HCID 21709030, 화합물

HRID 1890144
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HRID 1890144 반응식
O=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[S:5][CH:4]([C:12]([OH:14])=[O:13])[CH2:3]1.[C:15]1([NH:21]N)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[CH3:23][CH2:24]O>OS(O)(=O)=O>[CH2:23]([O:14][C:12]([CH:4]1[C:3]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[NH:21][C:2]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[S:5]1)=[O:13])[CH3:24]
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참가 물질

5

반응물 3

HCID 702EthanolHCID 7516PhenylhydrazineHCID 118391884-Oxothiochromane-2-carboxylic acid

생성물 1

HCID 21709030HCID 21709030, 화합물수율 51%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 4-oxo-thiochroman-2-carboxylic acid (3 g, 14 mmol) and phenyl hydrazine (1.4 ml, 14 mmol) in EtOH (14 ml), H2SO4 (1.8 ml) was added, and the mixture was heated at reflux for 5 hr. The reaction was cooled to room temperature and the solid, which formed overnight, was filtered, washed with cold EtOH and cold Et2O to give 2.26 g (51%) of 6,11-dihydro-5-thia-11-aza-benzo[α]fluorene-6-carboxylic acid ethyl ester as a crème solid. 1H NMR (CDCl3) δ 8.47 (1H, br s), 7.53-7.58 (1H, m), 7.10-7.40 (7H, m), 5.00 (1H, s), 4.09 (2H, q), 1.15 (3H, t).

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 5 hr
  3. customthe solid, which formed overnight
  4. filtrationwas filtered
  5. washwashed with cold EtOH and cold Et2O

출처 및 근거

ORD 기록
ord-1a8b9acaa85342ffa6858cd7a29e1a2d
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08506932B2

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