Hydrochloric Acid → HCID 24777543, 화합물

HRID 1364458노트

반응식

HRID 1364458 반응식
[Sn](Cl)Cl.Cl.[CH3:5][O:6][C:7]1[CH:25]=[CH:24][C:10]([O:11][CH2:12][C:13]2[CH:20]=[CH:19][CH:18]=[C:17]([N+:21]([O-])=O)[C:14]=2[C:15]#[N:16])=[CH:9][CH:8]=1.[OH-].[K+]>>[NH2:21][C:17]1[CH:18]=[CH:19][CH:20]=[C:13]([CH2:12][O:11][C:10]2[CH:9]=[CH:8][C:7]([O:6][CH3:5])=[CH:25][CH:24]=2)[C:14]=1[C:15]#[N:16]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 24479Stannous ChlorideHCID 24777539HCID 24777539, 화합물

생성물 1

HCID 24777543HCID 24777543, 화합물수율 73%

반응 조건

온도
15 °C

실험 절차

To a cooled (15° C.) and stirred solution of tin (II) chloride (0.37 g, 1.65 mmol) and con. hydrochloric acid (2.0 mL) was added a solution of 2-(4-methoxyphenoxymethyl)-6-nitrobenzonitrile (100.0 mg, 0.35 mmol). The reaction mixture was slowly warmed to room temperature and stirred for 3 hours. The reaction mixture was poured on to crushed-ice and potassium hydroxide solution, stirred, extracted with dichloromethane, filtered and dried. Purification by silica gel chromatography (1% methanol in dichloromethane) yielded 65 mg of 2-amino-6-(4-methoxyphenoxymethyl)benzonitrile.

후처리

  1. temperatureThe reaction mixture was slowly warmed to room temperature
  2. additionThe reaction mixture was poured on
  3. stirringstirred
  4. extractionextracted with dichloromethane
  5. filtrationfiltered
  6. customdried
  7. customPurification by silica gel chromatography (1% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-73bf5eda52ed421bbb2ad82c6b441611
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07888366B2

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