Sodium Bicarbonate → HCID 22258010、化合物

HRID 1251579ノート

反応式

HRID 1251579 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-1eb0082c1b444b439aad8a07f95cb603
出典データセット
uspto-grants-2002_01
特許番号
US06342502B1

反応ノート

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