Sodium Bicarbonate → HCID 22258010、化合物

HRID 1611018ノート

反応式

HRID 1611018 の反応式
[BH4-].[Na+].[NH2:3][C:4]1[S:5][C:6]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:7][C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].C(=O)(O)[O-].[Na+]>CC(C)C(O)=O.O>[CH3:4][CH:8]([CH3:9])[CH2:7][NH:3][C:4]1[S:5][C:6]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:7][C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

6

反応物 3

HCID 516892Sodium BicarbonateHCID 3792137Ethyl 2-amino-5-benzylthiophene-3-carboxylateHCID 4311764Sodium borohydride

生成物 1

HCID 22258010HCID 22258010、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6590Isobutyric Acid溶媒

実験手順

Sodium borohydride (3.0 g) was added in 6 portions over 3 hours to a stirred solution of ethyl 2-amino-5-(phenylmethyl)thiophene-3-carboxylate in 2-methylpropanoic acid under nitrogen. The mixture was stirred at room temperature for 20 hours and was then diluted with water, neutralized with sodium bicarbonate and extracted with ethyl acetate four times. The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography, eluting with diethyl ether:isohexane (1:19) to give the subtitle compound (2.80 g).

後処理

  1. extractionextracted with ethyl acetate four times
  2. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography
  6. washeluting with diethyl ether:isohexane (1:19)

出典と根拠

ORDレコード
ord-6f0e3dc80e464515bcfff6f6f329ac9c
出典データセット
uspto-grants-2006_01
特許番号
US06984644B2

反応ノート

読み込み中…