Hydrochloric Acid → HCID 22762736, 화합물

HRID 1112722노트

반응식

HRID 1112722 반응식
[I:1][C:2]1[C:7]([OH:8])=[C:6]([CH2:9][NH2:10])[CH:5]=[C:4]([C:11]([CH3:14])([CH3:13])[CH3:12])[N:3]=1.[ClH:15]>C(O)C.CCOCC>[ClH:15].[ClH:15].[I:1][C:2]1[C:7]([OH:8])=[C:6]([CH2:9][NH2:10])[CH:5]=[C:4]([C:11]([CH3:14])([CH3:13])[CH3:12])[N:3]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 1943074-(Aminomethyl)-6-(1,1-dimethylethyl)-2-iodo-3-pyridinol

생성물 1

HCID 22762736HCID 22762736, 화합물수율 91%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

To a solution of 2-iodo-4-aminomethyl-6-(1,1-dimethylethyl)-3-pyridinol (4.8 g., 0.016 mole) in ethanol (50 ml.) is added 12N hydrochloric acid (3 ml.). The resulting solution is diluted slowly with ether (150 ml.) and cooled to 0°-5° C. whereupon a solid is deposited. The solid is collected, washed with ether and air-dried to give 2-iodo-4-aminomethyl-6-(1,1-dimethylethyl)-3-pyridinol dihydrochloride (5.4 g., 91%), m.p. 177°-179° C. with dec. Recrystallization from ether-ethanol-water (125:50:2; v:v:v) affords an analytical sample of the 2-iodo-4-aminomethyl-6-(1,1-dimethylethyl)-3-pyridinol dihydrochloride as colorless needles, m.p. 178°-179° C. with dec.

후처리

  1. temperaturecooled to 0°-5° C. whereupon a solid
  2. customThe solid is collected
  3. washwashed with ether
  4. customair-dried

출처 및 근거

ORD 기록
ord-1d52512cb9d445a7aaeff88c158c5597
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04123537

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