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Trifluoroacetic acid → HCID 71285901、化合物

HRID 246225
ノート
印刷プレビュー

反応式

HRID 246225 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]2([NH:12][C:13]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([C:24]5[C:32]6[C:27](=[CH:28][C:29]([F:33])=[CH:30][CH:31]=6)[N:26]([CH3:34])[N:25]=5)[N:22]=4)[N:17](COCC[Si](C)(C)C)[CH:16]=3)=[O:14])[CH2:11][CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.C(O)(C(F)(F)F)=O.CC(=O)OCC.C(N(CC)CC)C>ClCCl.CO>[Br:1][C:2]1[CH:3]=[C:4]([C:8]2([NH:12][C:13]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([C:24]5[C:32]6[C:27](=[CH:28][C:29]([F:33])=[CH:30][CH:31]=6)[N:26]([CH3:34])[N:25]=5)[N:22]=4)[NH:17][CH:16]=3)=[O:14])[CH2:9][CH2:10][CH2:11]2)[CH:5]=[CH:6][CH:7]=1
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 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 71285950HCID 71285950、化合物

生成物 1

HCID 71285901HCID 71285901、化合物収率 38%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

To a light brown solution of 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanylethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [1-(3-bromo-phenyl)-cyclobutyl]-amide (50 mg, 0.077 mmol) in dichloromethane (3 mL) was added an excess of TFA (1.2 mL, 15.4 mmol) at room temperature under nitrogen atmosphere. The resulting light brown solution was stirred for 4 h at which time TLC analysis (EA, Rf=0.35) indicated the absence of starting material. Then, the solvent was removed under vacuum and the residue was azeotroped with toluene to obtain a light brown solid. Then, this solid was treated with an excess of triethylamine (1.07 mL, 7.7 mmol) in methanol (3 mL) at room temperature under nitrogen atmosphere. The resulting suspension was stirred for 15 h and then the solvent was removed under vacuum. The residue was triturated with acetonitrile and the solids were collected by filtration and washed with acetonitrile. After drying in air, 15 mg (38%) of the 2-(6-fluoro-1-methyl-1H-indazol-3-yl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid [1-(3-bromo-phenyl)-cyclobutyl]-amide was isolated as a light yellow solid. LC-MS (M+H)+=519; 1H NMR (300 MHz, DMSO-d6) δ: 12.80 (br. s., 1H), 9.10 (s, 1H), 8.77 (s, 1H), 8.55 (dd, J=8.8, 5.5 Hz, 1H), 8.36 (s, 1H), 7.64-7.80 (m, 2H), 7.57 (d, J=7.8 Hz, 1H), 7.41 (d, J=7.8 Hz, 1H), 7.23-7.35 (m, 1H), 7.15 (t, J=8.2 Hz, 1H), 4.15 (s, 3H), 2.56-2.81 (m, 4H), 2.19 (d, J=8.5 Hz, 1H), 1.96 (d, J=8.3 Hz, 1H).

後処理

  1. customThen, the solvent was removed under vacuum
  2. customthe residue was azeotroped with toluene
  3. customto obtain a light brown solid
  4. customthe solvent was removed under vacuum
  5. customThe residue was triturated with acetonitrile
  6. filtrationthe solids were collected by filtration
  7. washwashed with acetonitrile
  8. customAfter drying in air

出典と根拠

ORDレコード
ord-001c211d453143d7b80ce59d66300937
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08658646B2

反応ノート

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