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2-Amino-6-(trifluoromethyl)benzoic acid → HCID 54486842、化合物

HRID 1056441
ノート
印刷プレビュー

反応式

HRID 1056441 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[C:3]=1[C:4](O)=[O:5].[H-].[H-].[H-].[H-].[Li+].[Al+3]>O1CCCC1>[NH2:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:12])([F:13])[F:14])[C:3]=1[CH2:4][OH:5]
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 27785082-Amino-6-(trifluoromethyl)benzoic acidHCID 21226445Aluminium lithium hydride2 回

生成物 1

HCID 54486842HCID 54486842、化合物収率 97%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-amino-6-(trifluoromethyl)benzoic acid (20 g, 97 mmol) was dissolved in tetrahydrofuran (120 mL) in a 3-neck RB flask equipped with an addition funnel and a condenser. The solution was cooled in an ice-water bath. LiAlH4 (83 mL, 166 mmol) (2M solution in THF) was then added dropwise. After all of the LiAlH4 solution was added, the reaction mixture was allowed to warm to room temperature and stirred at room temperature overnight. The reaction was then quenched by adding 10 mL of Water, then 10 mL of 15% NaOH and then 25 mL of Water. The salts were filtered off and the solvents were evaporated under vacuum. The product was used as is (18 g, 97% yield.

後処理

  1. customequipped with an addition funnel and a condenser
  2. temperatureThe solution was cooled in an ice-water bath
  3. customThe reaction was then quenched
  4. additionby adding 10 mL of Water
  5. filtrationThe salts were filtered off
  6. customthe solvents were evaporated under vacuum

出典と根拠

ORDレコード
ord-d2c9abc313334f12b8b680d62f767f92
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09397302B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート