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Acetic Acid → HCID 178469256, 화합물

HRID 1606541
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HRID 1606541 반응식
[CH2:1]([NH:5][C:6]1[C:11]([N+:12]([O-])=O)=[C:10]([SH:15])[N:9]=[C:8]([CH3:16])[C:7]=1[C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:2][CH2:3]C.[C:22](O)(=O)C>[Fe]>[NH2:12][C:11]1[C:6]([NH:5][CH:1]([CH2:2][CH3:3])[CH3:22])=[C:7]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:8]([CH3:16])=[N:9][C:10]=1[SH:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 178448823HCID 178448823, 화합물

생성물 1

HCID 178469256HCID 178469256, 화합물

시약·촉매·용매 1

HCID 23925Iron촉매

실험 절차

6.2 g. of 4-sec. butylamino-6-mercapto-2-methyl-5-nitropyridine-3-carboxylic acid, ethyl ester are dissolved in 50 ml. of acetic acid. Iron dust is added carefully at relufx temperature until the mixture is colorless. The excess iron is filtered off and the filtrate is evaporated to dryness. The oily residue is dissolved in 10 ml. of methanol and precipitated by the addition of aqueous ammonia to obtain 5-amino-4-sec.butylamino-6-mercapto-2-methylpyridine-3-carboxylic acid, ethyl ester, yield 3 g. (53%), m. p. 88°-89° (ethyl acetate).

후처리

  1. waitof 4-sec
  2. filtrationThe excess iron is filtered off
  3. customthe filtrate is evaporated to dryness
  4. dissolutionThe oily residue is dissolved in 10 ml
  5. customof methanol and precipitated by the addition of aqueous ammonia

출처 및 근거

ORD 기록
ord-15e59bded2404e17bdf140062c9e5a41
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03953461

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