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Trifluoroacetic acid → 11-Oxo-2,3,10,11-tetrahydro-1H-benzo[b]indeno[5,6-f] thiepin-7-carboxylic acid

HRID 1731625
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HRID 1731625 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([OH:13])=O)=[C:6]([S:14][C:15]2[CH:16]=[C:17]3[C:21](=[CH:22][CH:23]=2)[CH2:20][CH2:19][CH2:18]3)[CH:5]=1)([OH:3])=[O:2].FC(F)(F)C(O)=O>FC(F)(F)C(OC(=O)C(F)(F)F)=O>[O:13]=[C:11]1[C:23]2[CH:22]=[C:21]3[C:17](=[CH:16][C:15]=2[S:14][C:6]2[CH:5]=[C:4]([C:1]([OH:3])=[O:2])[CH:9]=[CH:8][C:7]=2[CH2:10]1)[CH2:18][CH2:19][CH2:20]3
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 13746688HCID 13746688, 화합물

생성물 1

HCID 1374668911-Oxo-2,3,10,11-tetrahydro-1H-benzo[b]indeno[5,6-f] thiepin-7-carboxylic acid

시약·촉매·용매 1

HCID 9845Trifluoroacetic anhydride용매

실험 절차

4-Carboxy-2-(5-indanylthio)phenylacetic acid (33.55 g, 0.102 mole) was added to trifluoroacetic acid (200 ml) and to the stirred suspension was added, slowly with stirring, trifluoroacetic anhydride (200 ml). After stirring the mixture for 48 hours at room temperature, the mixture was poured slowly onto ice (200 g), and the slurry was diluted to about 1 liter before collecting the crude product. The dried solid was stirred in suspension in acetonitrile for 45 minutes, refiltered and dried to yield 24.95 g.

후처리

  1. additionwas added
  2. stirringAfter stirring the mixture for 48 hours at room temperature
  3. additionthe mixture was poured slowly onto ice (200 g)
  4. additionthe slurry was diluted to about 1 liter
  5. custombefore collecting the crude product
  6. stirringThe dried solid was stirred in suspension in acetonitrile for 45 minutes
  7. customdried
  8. customto yield 24.95 g

출처 및 근거

ORD 기록
ord-2025782b97374d608bc03578350c0f35
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04622403

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