Hydrochloric Acid → HCID 178422421, 화합물

HRID 1781236노트

반응식

HRID 1781236 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([N+:9]([O-])=[O:10])[C:3]=1[NH:12][C:13](=[O:18])[CH2:14]C(=O)C.[OH-].[Na+].Cl>C(O)(C)C.O>[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]2[C:3]=1[N:12]=[C:13]([OH:18])[CH:14]=[N+:9]2[O-:10]

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 14798Sodium HydroxideHCID 19045060HCID 19045060, 화합물

생성물 1

HCID 178422421HCID 178422421, 화합물수율 91.2%

시약·촉매·용매 2

HCID 962Water용매2회HCID 3776Isopropanol용매

실험 절차

The title compound of Step B (11.75 g, 37.29 mmol) was suspended in a mixture of isopropanol (120 mL) and water (120 mL) at room temperature under a nitrogen atmosphere. A solution of sodium hydroxide (14.91 g of a 50% aqueous solution, 186.4 mmol) diluted with water (10 mL) was added dropwise to the mixture over 30 min. The mixture was allowed to stir at room temperature overnight. First, 1N hydrochloric acid and then concentrated hydrochloric acid were added dropwise to the reaction mixture until the pH was approximately 2. Solids were filtered from the reaction mixture. These solids were washed with water and then cold ethyl acetate to afford the title compound of Step C as a reddish-brown solid melting at 241°-243° C. (8.67 g, 91%). 1H NMR ((CD3)2SO): δ2.47 (s,3H), 7.69 (s, 1H), 7.81 (s, 1H), 8.12 (s, 1H), 8.9 (br s, 1H).

후처리

  1. additionwas added dropwise to the mixture over 30 min
  2. filtrationSolids were filtered from the reaction mixture
  3. washThese solids were washed with water

출처 및 근거

ORD 기록
ord-961ef8e0d2254aeeb0222653c66e30f3
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05633218

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