Water → 6-Acety-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

HRID 1734042

反応式

HRID 1734042 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[C:10]([C:14](=O)[CH2:15][Br:16])=[C:11]([CH3:13])[S:12][C:6]=2[CH2:5]1)(=[O:3])[CH3:2].O>C([SiH](CC)CC)C.FC(F)(F)C(O)=O>[C:1]([N:4]1[CH2:9][CH2:8][C:7]2[C:10]([CH2:14][CH2:15][Br:16])=[C:11]([CH3:13])[S:12][C:6]=2[CH2:5]1)(=[O:3])[CH3:2]

参加物

5

反応物 2

HCID 962WaterHCID 214719586-Acetyl-3-bromoacetyl-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine

生成物 1

HCID 214719356-Acety-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine収率 52.3%

試薬・触媒・溶媒 2

HCID 6422Trifluoroacetic acid溶媒HCID 12052Triethylsilane溶媒

実験手順

A mixture of 28 g of 6-acetyl-3-bromoacetyl-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine in 42 ml of triethylsilane and 140 ml of trifluoroacetic acid was stirred at room temperature for 5 hours. The mixture was poured into water, made alkaline and extracted with ethyl acetate. The organic layer was washed with water, dried and concentrated. To the residue was added isopropyl ether and the precipitated crystals were collected by filtration to give 14 g of 6-acetyl-3-(2-bromoethyl)-4,5,6,7-tetrahydro-2-methylthieno[2,3-c]pyridine as white crystals, m.p. 93°-95° C.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated
  5. additionTo the residue was added isopropyl ether
  6. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-54977645a3514bc2aa29664f22a1d46a
出典データセット
uspto-grants-1996_07
特許番号
US05532240

関連ノート

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