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

HRID 1111619

반응식

HRID 1111619 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-8af6e775d9cb46f4831b64f9663c70d1
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04118397

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