Chloroacetamide → 10-Hydroxy-5,5-dimethyl-8-(1,2-dimethylheptyl)-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridine-2-acetamide

HRID 261731

反応式

HRID 261731 の反応式
Cl[CH2:2][C:3]([NH2:5])=[O:4].[OH:6][C:7]1[C:12]2[C:13]3[CH2:14][NH:15][CH2:16][CH2:17][C:18]=3[C:19]([CH3:22])([CH3:21])[O:20][C:11]=2[CH:10]=[C:9]([CH:23]([CH3:31])[CH:24]([CH3:30])[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH:8]=1.C(N(CC)CC)C>CN(C)C=O>[OH:6][C:7]1[C:12]2[C:13]3[CH2:14][N:15]([CH2:2][C:3]([NH2:5])=[O:4])[CH2:16][CH2:17][C:18]=3[C:19]([CH3:21])([CH3:22])[O:20][C:11]=2[CH:10]=[C:9]([CH:23]([CH3:31])[CH:24]([CH3:30])[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH:8]=1

参加物

5

反応物 3

HCID 6580ChloroacetamideHCID 8471TriethylamineHCID 2135435H-(1)Benzopyrano(4,3-c)pyridine, 1,2,3,4-tetrahydro-5,5-dimethyl-8-(1,2-dimethylheptyl)-10-hydroxy-

生成物 1

HCID 2132113810-Hydroxy-5,5-dimethyl-8-(1,2-dimethylheptyl)-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridine-2-acetamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of 1.03 g (0.011 mole) of 2-chloroacetamide in 8 ml of dimethylformamide was added dropwise to a stirred solution of 3.57 g (0.01 mole) of 10-hydroxy-5,5-dimethyl-8-(1,2-dimethylheptyl)-1,2,3,4-tetrahydro-5H-[1]benzopyrano[4,3-c]pyridine in 12 ml of dimethylformamide and 1.11 g (0.011 mole) of triethylamine. After stirring for 17 hours, the mixture was diluted with 20 ml. of water and extracted with ether. The combined ether extracts were washed with water, dried over anhydrous sodium sulfate, and evaporated in vacuo. The residue was recrystallized from acetonitrile, m.p. 165°-168°.

後処理

  1. additionthe mixture was diluted with 20 ml
  2. extractionof water and extracted with ether
  3. washThe combined ether extracts were washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated in vacuo
  6. customThe residue was recrystallized from acetonitrile, m.p. 165°-168°

出典と根拠

ORDレコード
ord-2d78b87b313a4731bf0a3aba2c2ff434
出典データセット
uspto-grants-1979_05
特許番号
US04152327

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