Triethylamine → HCID 178483602, 화합물

HRID 406577

반응식

HRID 406577 반응식
[CH3:1][NH:2][C:3]([CH3:9])=[CH:4][C:5]([O:7][CH3:8])=[O:6].C(N(CC)CC)C.[Cl:17][C:18]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21]>C1(C)C=CC=CC=1>[Cl:17][C:18]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:19]=1[C:20](=[O:21])[C:4](=[C:3]([NH:2][CH3:1])[CH3:9])[C:5]([O:7][CH3:8])=[O:6]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2734182Methyl 3-(methylamino)but-2-enoate2회HCID 27365462-Chloro-4-fluorobenzoyl chloride

생성물 1

HCID 178483602HCID 178483602, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
2.5 °C

실험 절차

To a mixture of methyl 3-(methylamino)-2-butenoate (i.e. the product of Step A) (10.25 g, 79.43 mmol) and triethylamine (13.26 mL, 9.63 g, 95.31 mmol) in toluene (125 mL) at 0° C. was added dropwise 2-chloro-4-fluorobenzoyl chloride (15.25 g, 79.48 mol) in toluene (25 mL) over 30 minutes while maintaining the temperature of the reaction mixture between about 0 to 5° C. The reaction mixture was allowed to warm to room temperature and stirred over night. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The resulting dark yellow oil was triturated with hexanes and filtered to provide the title compound as a white solid (15.91 g).

후처리

  1. temperatureto warm to room temperature
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe resulting dark yellow oil was triturated with hexanes
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-c2780f1beab64aee9f3d1542d987565d
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754115B2

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