Sodium Hydroxide → HCID 178515324, 화합물

HRID 627472

반응식

HRID 627472 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([I:11])=[CH:7][C:3]=1[C:4]([OH:6])=O.[F:12][C:13]([F:24])([F:23])[C:14](=O)[CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.CS(O)(=O)=O.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[OH-].[Na+].[NH4+].[OH-]>C(Cl)Cl>[I:11][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][CH:9]=1)[N:1]=[C:14]([C:13]([F:23])([F:24])[F:12])[C:15]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[C:4]2[OH:6]

참가 물질

7

반응물 5

HCID 14798Sodium HydroxideHCID 14923Ammonium HydroxideHCID 72911Benzoic acid, 2-amino-5-iodo-HCID 2229581,1,1-Trifluoro-3-phenyl-2-propanone2회HCID 86584057Phosphorus Pentoxide-Methanesulfonic Acid

생성물 1

HCID 178515324HCID 178515324, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
100 °C

실험 절차

A mixture of 2-amino-5-iodobenzoic acid (5.20 g, 19.8 mmol), 1,1,1-trifluoro-3-phenylpropan-2-one (3.95 g, 21.0 mmol), and Eaton's reagent (12 mL) in a sealed tube was heated at 100° C. for 2 hours. More 1,1,1-trifluoro-3-phenylpropan-2-one (1.60 g, 8.50 mmol) was added and the mixture was heated for another 2 hours. The reaction was then cooled to room temperature, ice water was added, and the mixture was stirred vigorously for about 20 min. 50% NaOH and conc. NH4OH solution were added until pH was 9. Some gummy dark brown material formed. After the addition of CH2Cl2, the gummy material became fluffy solid. This solid was filtered, washed with water and Et2O, and air dried to give the title compound.

후처리

  1. temperaturethe mixture was heated for another 2 hours
  2. temperatureThe reaction was then cooled to room temperature
  3. customSome gummy dark brown material formed
  4. filtrationThis solid was filtered
  5. washwashed with water and Et2O, and air
  6. customdried

출처 및 근거

ORD 기록
ord-1929ab8ba3eb4739a08d589c4e9fc9ad
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309222B2

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