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Sodium Thiosulfate Pentahydrate → 2-(2-(4-acetyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide

HRID 1162762
ノート
印刷プレビュー

反応式

HRID 1162762 の反応式
[OH:1][CH:2]([C:4]1[C:5]([C:25]([F:28])([F:27])[F:26])=[N:6][N:7]([CH2:9][C:10]([NH:12][C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([NH2:24])=[O:23])=[O:11])[CH:8]=1)[CH3:3].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.O.O.O.O.O.S([O-])([O-])(=O)=S.[Na+].[Na+].C(=O)(O)[O-].[Na+]>C(Cl)Cl.O.C(OCC)C>[C:2]([C:4]1[C:5]([C:25]([F:26])([F:28])[F:27])=[N:6][N:7]([CH2:9][C:10]([NH:12][C:13]2[S:17][C:16]3[CH2:18][CH2:19][CH2:20][CH2:21][C:15]=3[C:14]=2[C:22]([NH2:24])=[O:23])=[O:11])[CH:8]=1)(=[O:1])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 61475Sodium Thiosulfate PentahydrateHCID 159087TriacetoxyperiodinaneHCID 516892Sodium BicarbonateHCID 236488982-(2-(4-(1-hydroxyethyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide

生成物 1

HCID 595205152-(2-(4-acetyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

To 2-(2-(4-(1-hydroxyethyl)-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetamido)-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxamide (1.4 g, 3.36 mmol) in DCM (17 mL) was added a 15 wt % Dess-Martin periodinane in DCM solution (9.51 g, 6.99 mL, 3.36 mmol). The reaction was blanketed with argon and allowed to stir at RT for 6 h. Sodium thiosulfate pentahydrate (5.84 g, 23.53 mmol) was dissolved in water (20 mL) and mixed with saturated aqueous sodium bicarbonate (40 mL) before addition to the reaction mixture. The reaction mixture was allowed to stir for 40 min before the addition of diethyl ether. The aqueous was separated and extracted with diethyl ether (×3). The organics were combined and washed with water (×2) and brine (×1) before drying over MgSO4. The solvent was removed in vacuo to give the title compound as an off white solid (1.2 g, 2.90 mmol, 86%).

後処理

  1. customThe aqueous was separated
  2. extractionextracted with diethyl ether (×3)
  3. washwashed with water (×2) and brine (×1)
  4. dry with materialbefore drying over MgSO4
  5. customThe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-422b19c594c4419a8a86fecc30633b99
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820707B2

反応ノート

読み込み中…

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