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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
ノート
印刷プレビュー

反応式

HRID 1731625 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 13746688HCID 13746688、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 9845Trifluoroacetic anhydride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2025782b97374d608bc03578350c0f35
出典データセット
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04622403

反応ノート

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