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Trifluoroacetic acid → HCID 89704800、化合物

HRID 929005
ノート
印刷プレビュー

反応式

HRID 929005 の反応式
[NH2:1][C:2]1[C:11]([S:12]CC2C=CC(OC)=CC=2)=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([NH:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[F:29])[C:3]=1[F:30].C(O)(C(F)(F)F)=O>C1(OC)C=CC=CC=1>[NH2:1][C:2]1[C:11]([SH:12])=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[C:4]([NH:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[F:29])[C:3]=1[F:30]
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 89704787HCID 89704787、化合物

生成物 1

HCID 89704800HCID 89704800、化合物収率 75%

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

To a solution of methyl 4-amino-3-fluoro-2-((2-fluorophenyl)amino)-5-((4-methoxybenzyl)thio)benzoate (9.79 g, 22.7 mmol) in anisole (12 mL) was added CF3COOH (20 mL). After stirring at ambient temperature for 23 h, the solvent was removed in vacuo. To the residue was added water (30 mL). The mixture was neutralized with 25% aqueous ammonia and extracted with ethyl acetate (100 mL×3). The combined organic layer was washed with water (100 mL×3) and brine (100 mL) sequentially, dried over Na2SO4, filtered and concentrated to give the desired product (white solid, 5.28 g, 75% yield). The product was used directly in the next step without further purification.

後処理

  1. customthe solvent was removed in vacuo
  2. additionTo the residue was added water (30 mL)
  3. extractionextracted with ethyl acetate (100 mL×3)
  4. washThe combined organic layer was washed with water (100 mL×3) and brine (100 mL) sequentially
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-f9fd9e83c9ac4e76a3a81a91daf7b55a
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290468B2

反応ノート

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