Hydrochloric Acid → 3-(2-Anilinothiazol-4-yl)allyl alcohol

HRID 2107266노트

반응식

HRID 2107266 반응식
CCCCCC.[H-].C([Al+]CC(C)C)C(C)C.[NH:17]([C:24]1[S:25][CH:26]=[C:27]([CH:29]=[CH:30][C:31](OCC)=[O:32])[N:28]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl>O1CCCC1.CO>[NH:17]([C:24]1[S:25][CH:26]=[C:27]([CH:29]=[CH:30][CH2:31][OH:32])[N:28]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 21225700DiisobutylaluminumhydrideHCID 54052926Ethyl 3-(2-anilinothiazol-4-yl)acrylate

생성물 1

HCID 538556963-(2-Anilinothiazol-4-yl)allyl alcohol

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
-50 °C

실험 절차

58 ml of a 1M hexane solution of diisobutyl aluminum hydride was added dropwise at -60° C. to a solution of 4 g of ethyl 3-(2-anilinothiazol-4-yl)acrylate (prepared by the procedure described in Preparation 48) in 40 ml of tetrahydrofuran. The resulting mixture was stirred at -50° C. for 2 hours, then the excess of the reducing reagent was decomposed with 90% aqueous methanol. The mixture was then neutralized with 3N hydrochloric acid and extracted with ethyl acetate. After the extract was dried over anhydrous sodium sulfate. the solvent was evaporated off under reduced pressure, giving crude 3-(2-anilinothiazol-4-yl)allyl alcohol.

후처리

  1. customprepared by the procedure
  2. extractionextracted with ethyl acetate
  3. dry with materialAfter the extract was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated off under reduced pressure

출처 및 근거

ORD 기록
ord-b475f0aec9064786b9d13a3a4ce47621
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04933355

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