Triethylamine → HCID 22715001, 화합물

HRID 352013노트

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HRID 352013 반응식
[Cl:1][C:2]1[C:7]([NH2:8])=[C:6]([NH:9][CH2:10][CH:11]([CH3:13])[CH3:12])[CH:5]=[C:4]([CH3:14])[N:3]=1.C(N(CC)CC)C.[CH2:22]([O:24][CH2:25][C:26](Cl)=[O:27])[CH3:23]>ClCCl>[Cl:1][C:2]1[C:7]([NH:8][C:26](=[O:27])[CH2:25][O:24][CH2:22][CH3:23])=[C:6]([NH:9][CH2:10][CH:11]([CH3:12])[CH3:13])[CH:5]=[C:4]([CH3:14])[N:3]=1

참가 물질

5

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HCID 8471TriethylamineHCID 84189Ethoxyacetyl chlorideHCID 227150032-Chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine

생성물 1

HCID 22715001HCID 22715001, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

Anhydrous dichloromethane (750 ml) and 2-chloro-N4-(2-methylpropyl)-6-methylpyridin-3,4-diamine (18.84 g) were combined and cooled to 0° C. Triethylamine (12.9 ml) was added dropwise to the resulting mixture, and then ethoxyacetyl chloride (11.34 g) dissolved in anhydrous dichloromethane (50 ml) was added slowly to the resulting mixture, which turned dark. After two hours the dark mixture was allowed to warm to room temperature. TLC analysis of the reaction mixture indicated completion, and the solvent was removed under reduced pressure. The resulting yellow solid was dissolved in chloroform, and the resulting solution was washed with water. The organic layer was dried with magnesium sulfate and concentrated to a dark brown oil (27.75 g) under reduced pressure. NMR analysis of the oil indicated desired product of suitable purity for use in the next step.

후처리

  1. additionwas added slowly to the resulting mixture, which
  2. temperatureto warm to room temperature
  3. customthe solvent was removed under reduced pressure
  4. dissolutionThe resulting yellow solid was dissolved in chloroform
  5. washthe resulting solution was washed with water
  6. dry with materialThe organic layer was dried with magnesium sulfate
  7. concentrationconcentrated to a dark brown oil (27.75 g) under reduced pressure

출처 및 근거

ORD 기록
ord-ca1589a51e0d4996bf9068ed833c9673
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06743920B2

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