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Potassium Iodide → 2-Amino-3-carboethoxy-6-(3-phenyl)propyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine

HRID 325071
ノート
印刷プレビュー

反応式

HRID 325071 の反応式
[NH2:1][C:2]1[S:10][C:5]2[CH2:6][NH:7][CH2:8][CH2:9][C:4]=2[C:3]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12].[C:16]1([CH2:22][CH2:23][CH2:24]Br)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[NH2:1][C:2]1[S:10][C:5]2[CH2:6][N:7]([CH2:24][CH2:23][CH2:22][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:8][CH2:9][C:4]=2[C:3]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 12503(3-Bromopropyl)benzeneHCID 212359Thieno(2,3-c)pyridine-3-carboxylic acid, 4,5,6,7-tetrahydro-2-amino-, ethyl ester,

生成物 1

HCID 224645562-Amino-3-carboethoxy-6-(3-phenyl)propyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine収率 51.2%

試薬・触媒・溶媒 1

HCID 1140
Toluene
溶媒

実験手順

10.0 g (44.2 mmol) of 2-amino-3-carboethoxy-4,5,6,7-tetra-hydrothieno[2,3-c)pyridine [sic] in 100 ml of toluene were mixed with 9.0 g (45 mM) of 1-phenyl-3-bromopropane, 400 mg of potassium iodide and 6.1 g (44.2 mmol) of finely powdered potassium carbonate and refluxed for 6 h. The residue after concentration in a rotary evaporator was taken up in water, adjusted to pH=10 and extracted twice with methylene chloride. The crude product after drying and concentration of the organic phase was extracted by stirring in 50 ml of isopropanol. The pale solid was filtered off with suction and washed with isopropanol. 7.8 g (51%) of product with melting point 108-110° C. were isolated.

後処理

  1. temperaturerefluxed for 6 h
  2. concentrationThe residue after concentration
  3. customin a rotary evaporator
  4. extractionextracted twice with methylene chloride
  5. dry with materialThe crude product after drying
  6. extractionconcentration of the organic phase was extracted
  7. filtrationThe pale solid was filtered off with suction
  8. washwashed with isopropanol

出典と根拠

ORDレコード
ord-343c7c476ae244d18c1c4f74fe4e0b7d
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06222034B1

反応ノート

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