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Water → HCID 13344846, 화합물

HRID 485045
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HRID 485045 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH2:18][C:19]#[CH:20])[C:9]1[S:10][CH:11]=[C:12]([C:14](OC)=[O:15])[N:13]=1.O>O1CCCC1>[CH3:7][N:8]([CH2:18][C:19]#[CH:20])[C:9]1[S:10][CH:11]=[C:12]([CH2:14][OH:15])[N:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 13344843HCID 13344843, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 13344846HCID 13344846, 화합물수율 86.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Lithium aluminum hydride (900 mg) was added to anhydrous tetrahydrofuran (20 ml) and a solution of 2-(N-methyl-2-propynylamino)-4-methoxycarbonylthiazole (h) (5.0 g) in tetrahydrofuran (30 ml) was added dropwise thereto with stirring under ice-cooling. The mixture was refluxed for 2 hours, to which water was carefully added under ice-cooling, and evaporated to remove the tetrahydrofuran. The residue was extracted with chloroform. The extract was washed with water, dried and recrystallized from ether-hexane to give 2-(N-methyl-2-propynylamino)-4-hydroxymethylthiazole (i) (3.75 g, yield 86.5%): mp. 69°-70° C.

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후처리

  1. temperaturecooling
  2. additionwas carefully added under ice-
  3. temperaturecooling
  4. customevaporated
  5. customto remove the tetrahydrofuran
  6. extractionThe residue was extracted with chloroform
  7. washThe extract was washed with water
  8. customdried
  9. customrecrystallized from ether-hexane

출처 및 근거

ORD 기록
ord-3603e4c08e92433fa43e250b1ace144c
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04535088

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