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Methylhydrazine → HCID 178486239, 화합물

HRID 904809
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HRID 904809 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[C:9]([OH:10])=[C:8]([C:11]#[N:12])[O:7][C:6]=2[CH:13]=1.[CH3:14][NH:15][NH2:16]>C1C=CC=CC=1>[CH3:14][NH:15][NH:16][C:11]([C:8]1[O:7][C:6]2[CH:13]=[CH:2][CH:3]=[CH:4][C:5]=2[C:9]=1[OH:10])=[NH:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 132821406-Chloro-3-hydroxy-1-benzofuran-2-carbonitrile

생성물 1

HCID 178486239HCID 178486239, 화합물수율 43.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

3-Hydroxybenzo[b]furo-2-carbonitrile (1.40 g, 8.8 mmol, described in Example 3) was dissolved with heating in benzene (50 mL) and methyl hydrazine (1 mL, ca. 19 mmol) was added. The solution was stirred and refluxed for 2 hr and evaporated to dryness. The pasty residue (ca. 2 g) was applied in chloroform solution to chromatography on neutral alumina. Elution with 2% MeOH in CHCl3 (v/v) gave 3-hydroxybenzo[b]furan-2-carboximidic acid, 2-methylhydrazide (0.79 g): IR (CHCl3) 3510, 3480, 3450, 3200, 1635 and 1595 cm-1 ; and NMR (CDCl3) δ2.65 (3H, s), 5.7 (3H, broad), ca. 7.4 (1H, br), 7.2 (3H, m) and 7.75 (1H, d).

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후처리

  1. temperaturerefluxed for 2 hr
  2. customevaporated to dryness
  3. washElution with 2% MeOH in CHCl3 (v/v)

출처 및 근거

ORD 기록
ord-4db77d66eaae46cf9ba7e2533756134c
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04420476

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