Methyl 2-nitrobenzoate → 3-(1-Pyrrolidinyl)-4-phenoxy-5-amino-benzoic acid methyl ester

HRID 839055

반응식

HRID 839055 반응식
COC(=O)C1C=CC=CC=1[N+]([O-])=O.[CH3:14][O:15][C:16](=[O:38])[C:17]1[CH:22]=[C:21]([N+:23]([O-])=O)[C:20]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[C:19]([N:33]2[CH2:37][CH2:36][CH2:35][CH2:34]2)[CH:18]=1>O1CCOCC1.[Ni]>[CH3:14][O:15][C:16](=[O:38])[C:17]1[CH:22]=[C:21]([NH2:23])[C:20]([O:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)=[C:19]([N:33]2[CH2:34][CH2:35][CH2:36][CH2:37]2)[CH:18]=1

참가 물질

5

반응물 2

HCID 69072Methyl 2-nitrobenzoateHCID 124983403-(1-Pyrrolidinyl)-4-phenoxy-5-nitrobenzoic acid methyl ester

생성물 1

HCID 124983413-(1-Pyrrolidinyl)-4-phenoxy-5-amino-benzoic acid methyl ester

시약·촉매·용매 2

HCID 935Nickel촉매HCID 312751,4-Dioxane용매

실험 절차

A solution of 30 g of the nitrobenzoic acid methyl ester obtained according to (b) in 500 ml of dioxane is hydrogenated catalytically in the presence of Raney nickel. After completion of the absorption of hydrogen, the whole is filtered and the filtrate is concentrated. The residue yields, on recrystallization from methanol, the desired compound in the form of colourless crystals melting at 153°-156° C in a very good yield.

후처리

  1. customAfter completion of the absorption of hydrogen
  2. filtrationthe whole is filtered
  3. concentrationthe filtrate is concentrated
  4. customThe residue yields, on recrystallization from methanol

출처 및 근거

ORD 기록
ord-03670224eb4545edb7313e82c3c53f75
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093735

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