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Hydrochloric Acid → 1-[4-(9-Phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)phenyl]ethanamine

HRID 1678749
ノート
印刷プレビュー

反応式

HRID 1678749 の反応式
CC(S([NH:7][CH:8]([C:10]1[CH:15]=[CH:14][C:13]([C:16]2[C:25]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)=[CH:24][C:23]3[C:22]4=[N:32][N:33]=[CH:34][N:21]4[CH:20]=[CH:19][C:18]=3[N:17]=2)=[CH:12][CH:11]=1)[CH3:9])=O)(C)C.Cl.O>CO>[C:26]1([C:25]2[C:16]([C:13]3[CH:12]=[CH:11][C:10]([CH:8]([NH2:7])[CH3:9])=[CH:15][CH:14]=3)=[N:17][C:18]3[CH:19]=[CH:20][N:21]4[CH:34]=[N:33][N:32]=[C:22]4[C:23]=3[CH:24]=2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 594730512-Methyl-N-{1-[4-(9-phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)phenyl]ethyl}propane-2-sulfinamide

生成物 1

HCID 159792751-[4-(9-Phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)phenyl]ethanamine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of 2-methyl-N-{1-[4-(9-phenyl[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl)phenyl]ethyl}propane-2-sulfinamide (7-3, 180 mg, 0.38 mmol) in methanol (6 mL) was added conc. HCl (1.5 mL). After 1 h, water was added and the mixture was washed with methylene chloride. The aqueous portion was basified with saturated sodium carbonate solution and extracted with methylene chloride. 2N HCl (5 mL) was added to the organic layer and the mixture was concentrated to a minimum volume. The crude product was purified using reverse phase preparative HPLC to give the title compound as a pale yellow solid. LRMS m/z (M+1) Calcd: 366.2. Found 366.3.

後処理

  1. washthe mixture was washed with methylene chloride
  2. extractionextracted with methylene chloride
  3. addition2N HCl (5 mL) was added to the organic layer
  4. concentrationthe mixture was concentrated to a minimum volume
  5. customThe crude product was purified

出典と根拠

ORDレコード
ord-15a84619b5334b36855689fd441b7c68
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08008317B2

反応ノート

読み込み中…

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