HCID 66650497, 화합물 → Amino-5-ethoxy-4-trifluoromethyl-benzonitrile

HRID 418145노트

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HRID 418145 반응식
[CH2:1]([O:3][C:4]1[C:5]([C:15]([F:18])([F:17])[F:16])=[CH:6][C:7]([N+:12]([O-])=O)=[C:8]([CH:11]=1)[C:9]#[N:10])[CH3:2]>CO.Cl.[Fe]>[NH2:12][C:7]1[CH:6]=[C:5]([C:15]([F:17])([F:18])[F:16])[C:4]([O:3][CH2:1][CH3:2])=[CH:11][C:8]=1[C:9]#[N:10]

참가 물질

5

반응물 1

HCID 66650497HCID 66650497, 화합물

생성물 1

HCID 66650419Amino-5-ethoxy-4-trifluoromethyl-benzonitrile수율 84%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 313Hydrochloric Acid용매HCID 887Methanol용매

반응 조건

온도
50 °C

실험 절차

Iron powder (40.96 g, 733 mmol) was added in small portions over 5 min to a stirred suspension of finely grinded 5-ethoxy-2-nitro-4-trifluoromethyl-benzonitrile from step 3 (42.79 g, 164.5 mmol) in MeOH (85 mL) and conc. HCl (102 mL) with water bath cooling keeping the internal temperature at 40-50° C. The resulting mixture was stirred for further 1 h at ca. 50° C. and then poured into ice cold H2O (700 mL). The precipitate was filtered, washed with water, dried, and dissolved in boiling EtOH (800 mL), activated carbon (ca. 10 g) was added, the mixture was refluxed for 45 min, the hot solution was filtered and evaporated to dryness to leave a yellow solid (31.81 g, 84%), which was used without further purification. MS (EI) 230.1 [M].

후처리

  1. temperaturecooling
  2. customat 40-50° C
  3. filtrationThe precipitate was filtered
  4. washwashed with water
  5. customdried
  6. dissolutiondissolved
  7. additionwas added
  8. temperaturethe mixture was refluxed for 45 min
  9. filtrationthe hot solution was filtered
  10. customevaporated to dryness

출처 및 근거

ORD 기록
ord-c270145300d541d69037e2f8bbf0d950
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093263B2

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