Hydrochloric Acid → 2-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethanamine

HRID 455536노트

반응식

HRID 455536 반응식
[C:1]([CH2:3][CH:4]1[O:9][C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[O:6][CH2:5]1)#[N:2].Cl>C1COCC1>[O:9]1[C:8]2[CH:10]=[CH:11][CH:12]=[CH:13][C:7]=2[O:6][CH2:5][CH:4]1[CH2:3][CH2:1][NH2:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 2675312-(2,3-Dihydro-1,4-benzodioxin-2-yl)acetonitrile

생성물 1

HCID 556482-(2,3-Dihydro-1,4-benzodioxin-2-yl)ethanamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The 2-cyanomethyl-(2,3 dihydrobenzo[1,4]dioxine) was dissolved in THF (50 mL) and 1M BH3 in THF (80 mL, 80 mmol) was added and the reaction mixture refluxed for 5 h, then stirred at ambient temperature for 16 h. With ice bath cooling, 2N HCl was added until pH=1.0 was achieved. The reaction mixture was then stirred for 1 h at room temperature and evaporated in vacuo to yield an oil. The oil was partitioned between 3N NaOH and diethyl ether, and the diethyl ether solution was washed with brine, dried (Na2SO4) and evaporated in vacuo to yield crude 2-(2,3 dihydrobenzo[1,4]dioxin-2-yl)ethylamine.

후처리

  1. temperaturethe reaction mixture refluxed for 5 h
  2. temperatureWith ice bath cooling
  3. stirringThe reaction mixture was then stirred for 1 h at room temperature
  4. customevaporated in vacuo
  5. customto yield an oil
  6. customThe oil was partitioned between 3N NaOH and diethyl ether
  7. washthe diethyl ether solution was washed with brine
  8. dry with materialdried (Na2SO4)
  9. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-23779fdc1e0c43079946be52b228c655
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497298B2

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