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Sodium borohydride → (4-(Trifluoromethyl)-1,3-thiazol-2-yl)methanol

HRID 1497399
ノート
印刷プレビュー

反応式

HRID 1497399 の反応式
[BH4-].[Na+].[F:3][C:4]([F:16])([F:15])[C:5]1[N:6]=[C:7]([C:10](OCC)=[O:11])[S:8][CH:9]=1>CO>[F:16][C:4]([F:3])([F:15])[C:5]1[N:6]=[C:7]([CH2:10][OH:11])[S:8][CH:9]=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 4311764Sodium borohydrideHCID 23560697Ethyl 4-(trifluoromethyl)thiazole-2-carboxylate

生成物 1

HCID 23560688(4-(Trifluoromethyl)-1,3-thiazol-2-yl)methanol収率 83.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium tetrahydroborate (840 mg) was added to a solution of ethyl 4-(trifluoromethyl)-1,3-thiazole-2-carboxylate (2.5 g) in methanol (15 ml) at 0° C., and the mixture was stirred at the same temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate) to give the title compound (1.7 g).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with water
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-c3705374585541c890b69f84e6009047
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09199963B2

反応ノート

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