Sodium hydride → HCID 178514754、化合物

HRID 2040262ノート

反応式

HRID 2040262 の反応式
[Si]([O:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([CH2:15][OH:16])[CH2:11][CH2:10]1)(C(C)(C)C)(C)C.[Cl:17][C:18]1[CH:19]=[C:20]([S:25]([NH2:28])(=[O:27])=[O:26])[CH:21]=[CH:22][C:23]=1F.[H-].[Na+]>O1CCCC1>[Cl:17][C:18]1[CH:19]=[C:20]([S:25]([NH2:28])(=[O:26])=[O:27])[CH:21]=[CH:22][C:23]=1[O:16][CH2:15][C@H:12]1[CH2:11][CH2:10][C@H:9]([OH:8])[CH2:14][CH2:13]1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 75098833-Chloro-4-fluorobenzenesulfonamideHCID 178455322HCID 178455322、化合物

生成物 1

HCID 178514754HCID 178514754、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(Trans-4-(tert-butyldimethylsilyloxy)cyclohexyl)methanol (275 mg, prepared according to a procedures in WO 2008/124878) and 3-chloro-4-fluorobenzenesulfonamide (259 mg) in tetrahydrofuran (15 mL) were treated with sodium hydride (180 mg, 60%) overnight. The reaction was quenched with water (1 mL) and trifluoroacetic acid (4 mL) was added. The resulting mixture was stirred for 1 hour and concentrated. The residue was triturated with water and methanol to provide the title compound.

後処理

  1. customThe reaction was quenched with water (1 mL) and trifluoroacetic acid (4 mL)
  2. additionwas added
  3. concentrationconcentrated
  4. customThe residue was triturated with water and methanol

出典と根拠

ORDレコード
ord-24f8c9190aee49818fbb727d4995af7d
出典データセット
uspto-grants-2013_11
特許番号
US08580794B2

反応ノート

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