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Hydrazine hydrate (1:1) → 2-Amino-6-(2-phenoxyethoxy)benzamide

HRID 973065
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반응식

HRID 973065 반응식
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:5]=1[C:6]#[N:7])([O-])=O.[OH2:22].NN>C(O)C.[Ni]>[NH2:1][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:5]=1[C:6]([NH2:7])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 122648282-Nitro-6-(2-phenoxyethoxy)benzonitrile

생성물 1

HCID 122648352-Amino-6-(2-phenoxyethoxy)benzamide수율 50.2%

시약·촉매·용매 2

HCID 935Nickel촉매2회HCID 702Ethanol용매

실험 절차

The crystallized 2-nitro-6-(2-phenoxyethoxy)benzonitrile (5.82 g, 0.0205 mole) is stirred in 116 ml absolute ethanol at 50° C. and 3.62 ml. (0.0615 mole) 85 percent hydrazine hydrate is added, followed by small scoops of Raney nickel. The temperature is kept at 50°-60° C. while the Raney nickel is added, and after gas evolution and the exotherm ceases, the mixture is filtered through diatomaceous earth. The filter cake is washed with hot ethanol and the filtrate is concentrated, giving 2.804 g of 2-amino-6-(2-phenoxyethoxy)benzamide m.p. 127°-130° C.

후처리

  1. additionis added
  2. filtrationafter gas evolution and the exotherm ceases, the mixture is filtered through diatomaceous earth
  3. washThe filter cake is washed with hot ethanol
  4. concentrationthe filtrate is concentrated

출처 및 근거

ORD 기록
ord-8a60f5b1eee9409babffd974b53dd910
출처 데이터셋
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04054661

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