4-Nitroanthranilic acid → 2-Amino-4-nitrobenzoyl chloride

HRID 889437노트

반응식

HRID 889437 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4](O)=[O:5].S(Cl)([Cl:16])=O>>[NH2:1][C:2]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([Cl:16])=[O:5]

참가 물질

3

반응물 2

HCID 120764-Nitroanthranilic acidHCID 24386Thionyl Chloride

생성물 1

HCID 214891672-Amino-4-nitrobenzoyl chloride수율 119.8%

실험 절차

2-Amino-4-nitrobenzoic acid (15 g, 82 mmol) was refluxed with sulfurous dichloride (40 mL, 82 mmol) for 2.5 hours. The reaction mixture was cooled to room temperature and concentrated to give Intermediate 69A (19.7 g, 119%) as a brown oil. HPLC: Rt=2.323 (as methyl ester) min. (CHROMOLITH® column 4.6×50 mm eluting with 10-90% aqueous methanol over 4 min. containing 0.1% TFA, 4 mL/min., monitoring at 220 nm.). MS (ES): m/z=197 (as methyl ester) [M+H]+.

후처리

  1. concentrationconcentrated

출처 및 근거

ORD 기록
ord-af787e895f6b4bf089469efea35f5a1b
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252795B2

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