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

HRID 1448712
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HRID 1448712 반응식
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
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 23341602N-(3-Carbomethoxy-5-methyl-2-thienyl)-2-methylpropanamideHCID 23688289Lithium iodide (LiI), dihydrate

생성물 1

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

시약·촉매·용매 1

HCID 7953
2,4,6-Trimethylpyridine
용매
2회

실험 절차

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 5N-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.

후처리

  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

출처 및 근거

ORD 기록
ord-afad9c58544d494699d4c6e89ba2733c
출처 데이터셋
uspto-grants-1980_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04187232

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