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Ethanol → HCID 178521009、化合物

HRID 931223
ノート
印刷プレビュー

反応式

HRID 931223 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[N:8]=[C:7]([CH:9]=O)[CH:6]=[CH:5][CH:4]=1.Cl.Cl.[NH2:15][C:16]1[CH:17]=[CH:18][C:19]([N:23]2[CH2:28][CH2:27][CH2:26][C@@H:25]([C:29]([N:31]3[CH2:35][CH2:34][CH2:33][CH2:32]3)=[O:30])[CH2:24]2)=[N:20][C:21]=1[NH2:22].S(S([O-])=O)([O-])=O.[Na+].[Na+].C(O)C>O>[N:31]1([C:29]([C@@H:25]2[CH2:26][CH2:27][CH2:28][N:23]([C:19]3[N:20]=[C:21]4[NH:22][C:9]([C:7]5[CH:6]=[CH:5][CH:4]=[C:3]([C:2]([F:12])([F:11])[F:1])[N:8]=5)=[N:15][C:16]4=[CH:17][CH:18]=3)[CH2:24]2)=[O:30])[CH2:35][CH2:34][CH2:33][CH2:32]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 24489Sodium DithioniteHCID 147614746-(Trifluoromethyl)pyridine-2-carbaldehydeHCID 89854051(R)-(1-(5,6-Diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride2 回

生成物 1

HCID 178521009HCID 178521009、化合物収率 29%

試薬・触媒・溶媒 1

HCID 962
Water
溶媒

反応条件

温度
110 °C

実験手順

Into a tube was added 6-(trifluoromethyl)picolinaldehyde (150 mg, 0.47 mmol), (R)-(1-(6-amino-5-nitropyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone (Intermediate 1, Step 3) (82.2 mg, 0.47 mmol), sodium dithionite (310.7 mg, 1.78 mmol), ethanol (10 mL) and water (1.5 mL). The vessel was sealed and the reaction mixture was stirred at 110° C. for 16 h. The solvent was evaporated under reduced pressure and water was added to the resulting residue. The mixture was extracted with ethyl acetate, dried over sodium sulfate and concentrated under reduced pressure. The crude material was purified via preparative TLC to afford the title compound (50 mg, 29%) as a yellow solid. MS (ES+APCI) (M+H) 445.2; LCMS retention time 2.657 min (Method G).

後処理

  1. customThe vessel was sealed
  2. customThe solvent was evaporated under reduced pressure and water
  3. additionwas added to the resulting residue
  4. extractionThe mixture was extracted with ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe crude material was purified via preparative TLC

出典と根拠

ORDレコード
ord-06039163eacd4e4caa0ef925887c43c4
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296745B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート