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Trifluoroacetic acid → HCID 57520094、化合物

HRID 1528099
ノート
印刷プレビュー

反応式

HRID 1528099 の反応式
[F:1][C:2]([F:37])([F:36])[C:3]1[N:8]=[C:7]([NH:9][C:10](=[O:35])[NH:11][C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[C:19]([C:22]4[CH2:23][CH2:24][N:25](C(OC(C)(C)C)=O)[CH2:26][CH:27]=4)[CH:20]=3)[N:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH:25]1[CH2:26][CH:27]=[C:22]([C:19]2[CH:20]=[C:21]3[C:16](=[CH:17][CH:18]=2)[N:15]=[CH:14][CH:13]=[C:12]3[NH:11][C:10]([NH:9][C:7]2[CH:6]=[CH:5][CH:4]=[C:3]([C:2]([F:36])([F:37])[F:1])[N:8]=2)=[O:35])[CH2:23][CH2:24]1
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 57520093HCID 57520093、化合物

生成物 1

HCID 57520094HCID 57520094、化合物収率 80.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

0.2 g of tert-butyl 4-{4-[3-(6-trifluoromethyl-pyridin-2-yl)-ureido]-quinolin-6-yl}-3,6-dihydro-2H-pyridine-1-carboxylate (0.389 mmol) were dissolved in 0.6 ml DCM (yellow solution). 0.300 ml of TFA (3.89 mmol) were added and the reaction mixture was stirred for 2 h at RT. After evaporation of the solvent and excess TFA in vacuum, water was added to the residue, the acidic mixture extracted with ethyl acetate, the water phase adjusted to pH 9 with 1M NaOH and subsequently extracted three times with DCM. The combined DCM solutions were washed with a small amount of brine, dried over sodium sulphate and the solvent was removed in vacuum. 130 mg of the desired product were obtained as light yellow powder (yield: 81%).

後処理

  1. customAfter evaporation of the solvent and excess TFA in vacuum, water
  2. additionwas added to the residue
  3. extractionthe acidic mixture extracted with ethyl acetate
  4. extractionsubsequently extracted three times with DCM
  5. washThe combined DCM solutions were washed with a small amount of brine
  6. dry with materialdried over sodium sulphate
  7. customthe solvent was removed in vacuum

出典と根拠

ORDレコード
ord-e1b7751bd9c0472e9f8a8e0862e1abc4
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090592B2

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