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Hydrochloric Acid → 2-Methyl-N-(5-methylthiophen-2-yl)propanamide

HRID 27668
ノート
印刷プレビュー

反応式

HRID 27668 の反応式
C([C:5]1[CH:9]=[C:8]([CH3:10])[S:7][C:6]=1[NH:11][C:12](=[O:16])[CH:13]([CH3:15])[CH3:14])(OC)=O.O.O.[I-].[Li+].CCOCC.Cl>N1C(C)=CC(C)=CC=1C>[CH3:10][C:8]1[S:7][C:6]([NH:11][C:12](=[O:16])[CH:13]([CH3:14])[CH3:15])=[CH:5][CH:9]=1
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 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 23341602N-(3-Carbomethoxy-5-methyl-2-thienyl)-2-methylpropanamideHCID 23688289Lithium iodide (LiI), dihydrate

生成物 1

HCID 233416282-Methyl-N-(5-methylthiophen-2-yl)propanamide収率 86.7%

試薬・触媒・溶媒 1

HCID 7953
2,4,6-Trimethylpyridine
溶媒
2 回

実験手順

N-(3-Carbomethoxy-5-methyl-2-thienyl)-2-methylpropanamide (4.1 g, 0.017 mol), prepared by the method of Example 48, was dissolved in hot collidine (10 ml) and added to a mixture of lithium iodide dihydrate (10.1 g, 0.06 mol) in collidine (20 ml) kept under nitrogen. The reaction mixture was stirred under reflux for 48 hours, cooled and equilibrated between ether (3×50 ml) and 5 N-hydrochloric acid (50 ml). The ethereal solution was washed with water (25 ml), dried (Na2SO4) and evaporated to yield the required product as an off-white solid (2.7 g, 47%) m.p. 96°-97° C. The product was identical to the product described in Example 38.

後処理

  1. temperatureunder reflux for 48 hours
  2. temperaturecooled
  3. washThe ethereal solution was washed with water (25 ml)
  4. dry with materialdried (Na2SO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-20f01006fd414d4dab39ec0fa82bcd2b
出典データセット
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04222946

反応ノート

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