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2-(Trifluoromethyl)benzoic acid → HCID 58792452、化合物

HRID 1359944
ノート
印刷プレビュー

反応式

HRID 1359944 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:11]=[CH:10][CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.[CH3:14][C:15]([CH3:26])([CH3:25])[C:16]#[C:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[NH2:24].C(N(CC)C(C)C)(C)C.C1CN([P+](Br)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F>C(#N)C.C(OCC)(=O)C.O>[CH3:14][C:15]([CH3:26])([CH3:25])[C:16]#[C:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[NH:24][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[CH:11][C:3]=1[C:2]([F:1])([F:13])[F:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 98992-(Trifluoromethyl)benzoic acidHCID 81531DiisopropylethylamineHCID 2733179PyBroPHCID 140666562-(3,3-Dimethylbut-1-yn-1-yl)aniline

生成物 1

HCID 58792452HCID 58792452、化合物収率 38.4%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile
溶媒
HCID 22728543Water ethylacetate溶媒

実験手順

190 mg (1.0 mmol) of 2-trifluoromethylbenzoic acid, 178 mg (0.83 mmol) of 2-(3,3-dimethyl-but-1-ynyl)phenylamine, 215 mg (1.67 mmol) of N,N-diisopropylethylamine and 583 mg (1.25 mmol) of PyBrOP in 8 ml of acetonitrile were stirred at room temperature for 4 days. 10 ml of ethyl acetate/water 1:1 were added to the mixture and the organic phase was separated off and washed with 10 ml of saturated ammonium chloride solution and subsequently with 10 ml of water. Separation, concentration and drying of the organic phase gave 950 mg of crude product. Column-chromatographic purification on silica gel 60 (petroleum ether/ethyl acetate 10:1→ethyl acetate) gave 110 mg of N-[2-(3,3-dimethylbut-1-ynyl)phenyl]-2-trifluoromethylbenzamide [logP (pH 2.3)=4.55].

後処理

  1. customthe organic phase was separated off
  2. washwashed with 10 ml of saturated ammonium chloride solution and subsequently with 10 ml of water
  3. customSeparation, concentration
  4. customdrying of the organic phase
  5. customgave 950 mg of crude product
  6. customColumn-chromatographic purification on silica gel 60 (petroleum ether/ethyl acetate 10:1→ethyl acetate)

出典と根拠

ORDレコード
ord-bac27973fdab406487443dc0bc1a1514
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879760B2

反応ノート

読み込み中…

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