Nitric Acid → HCID 131728508, 화합물

HRID 2425087노트

반응식

HRID 2425087 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([CH3:21])[C:8]2[O:14][C:13]3[C:15]([Cl:19])=[CH:16][CH:17]=[CH:18][C:12]=3[CH2:11][S:10][C:9]=2[CH:20]=1)=[O:4].[N+:22]([O-])([OH:24])=[O:23].S(=O)(=O)(O)[OH:27]>>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[C:7]([CH3:21])[C:8]2[O:14][C:13]3[C:15]([Cl:19])=[CH:16][C:17]([N+:22]([O-:24])=[O:23])=[CH:18][C:12]=3[CH2:11][S:10](=[O:27])[C:9]=2[CH:20]=1)=[O:4]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 672474734-Chloro-6-methyl-11h-5-oxa-10-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid methyl ester

생성물 1

HCID 131728508HCID 131728508, 화합물

실험 절차

Compound of Example 15b (4.1 g, 12.8 mmol) was added to solution of nitrating mixture (nitric acid 200 mL and sulfuric acid 20 mL) at 0° C. and stirred for 18 h. The reaction mixture was poured slowly with stirring into ice water (200 mL). The solid separated was filtered, washed with water and dried to obtain the title compound. Yield: 2.5 g, (52%); 1H NMR (CDCl3, 300 MHz): δ 2.65 (s, 3H, CH3), 3.93 (s, 3H, OCH3), 4.57 (s, 2H, CH2), 8.16 (d, 2H, Ar), 8.35 (d, 2H, Ar); MS: m/e (ES−) 380 (M−1).

후처리

  1. additionThe reaction mixture was poured slowly
  2. customThe solid separated
  3. filtrationwas filtered
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-c0eefcb999d641e7a83fe6b08ec93bf0
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07964631B2

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