Allylamine → HCID 20718717, 화합물

HRID 1250621

반응식

HRID 1250621 반응식
[CH2:1]([NH2:4])[CH:2]=[CH2:3].Cl[C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1>O>[CH2:1]([NH:4][C:6]1[N:7]=[C:8]([NH:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:9]2[S:14][CH:13]=[C:12]([CH3:15])[C:10]=2[N:11]=1)[CH:2]=[CH2:3]

참가 물질

4

반응물 2

HCID 7853AllylamineHCID 183264882-Chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine

생성물 1

HCID 20718717HCID 20718717, 화합물수율 63.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

In 2.28 g (40.0 mmol) of allylamine was dissolved 250 mg (0.9 mmol) of 2-chloro-7-methyl-4-neopentylaminothieno[3,2-d]pyrimidine, and the resulting solution was heated in a sealed tube at 140° C. for 24 hours. After the reaction mixture was cooled, 100 ml of water was added thereto, followed by extraction with ethyl acetate (20 ml×3). The organic layer was washed with 20 ml of water and dried over anhydrous sodium sulfate, and then the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 165 mg (yield: 61.3%) of the title compound.

후처리

  1. temperatureAfter the reaction mixture was cooled
  2. extractionfollowed by extraction with ethyl acetate (20 ml×3)
  3. washThe organic layer was washed with 20 ml of water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)

출처 및 근거

ORD 기록
ord-f7636c58f46944e68fb38628c3653a80
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339089B2

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