Water → [2-(Trifluoromethyl)-1H-indol-3-yl]methanol

HRID 231836

反応式

HRID 231836 の反応式
[BH4-].[K+].[F:3][C:4]([F:17])([F:16])[C:5]1[NH:6][C:7]2[C:12]([C:13]=1[CH:14]=[O:15])=[CH:11][CH:10]=[CH:9][CH:8]=2.O1CCCC1.O>CCOCC>[F:17][C:4]([F:3])([F:16])[C:5]1[NH:6][C:7]2[C:12]([C:13]=1[CH2:14][OH:15])=[CH:11][CH:10]=[CH:9][CH:8]=2

参加物

6

反応物 4

HCID 962WaterHCID 8028Tetrahydrofuran2 回HCID 4192641Potassium borohydrideHCID 200321282-trifluoromethyl-3-formyl-(1H)-indole

生成物 1

HCID 20032113[2-(Trifluoromethyl)-1H-indol-3-yl]methanol収率 64.6%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

2 g of potassium borohydride were added in small fractions at +5° C. to a solution of 4.6 g of the product of Step A, 150 ml of tetrahydrofuran and 30 ml of water and the mixture was stirred for one hour. The mixture was allowed to return to ambient temperature and the tetrahydrofuran was eliminated under reduced pressure. The resulting mixture was diluted with ether, washed with water, dried and concentrated under reduced pressure. The residue was chromatographed over silica (eluent: hexaneethyl acetate 7-3) to obtain 3 g of 2-trifluoromethyl-(1H)-indol-3-yl methanol melting at 106° C.

後処理

  1. customto return to ambient temperature
  2. washwashed with water
  3. customdried
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was chromatographed over silica (eluent: hexaneethyl acetate 7-3)

出典と根拠

ORDレコード
ord-ad967951fb5a48f7bfe9f3319054f3fa
出典データセット
uspto-grants-1989_07
特許番号
US04849443

関連ノート

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