Hydrochloric Acid → 2,3-dihydro-1H-inden-1-ylmethanamine

HRID 414176노트

반응식

HRID 414176 반응식
B#B.[CH:3]1([C:12]([NH2:14])=O)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4]1.Cl>C1COCC1>[CH:3]1([CH2:12][NH2:14])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 1180992,3-dihydro-1H-indene-1-carboxamideHCID 6328200Diboron

생성물 1

HCID 143486922,3-dihydro-1H-inden-1-ylmethanamine수율 71%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 150 ml of diborane (1M in THF) in 250 ml of dry THF. Ten g of 1-indane carboxamide is slowly added. Reaction mixture is stirred at reflux for three hours, cooled to room temperature, and worked up by slowly adding 150 ml of 1N HCl. THF is distilled off under reduced pressure, the aqueous solution is brought to pH~13 by addition of NaOH. It is extracted with ethyl acetate (2×300 ml). The organic extract is washed with water (1×100 ml), dried over MgSO4, filtered, and evaporated to dryness affording 6.5 g (71%) of 1-indanylmethylamine. It was used as is in the next reaction.

후처리

  1. customReaction mixture
  2. temperatureat reflux for three hours
  3. distillationTHF is distilled off under reduced pressure
  4. additionthe aqueous solution is brought to pH~13 by addition of NaOH
  5. extractionIt is extracted with ethyl acetate (2×300 ml)
  6. extractionThe organic extract
  7. washis washed with water (1×100 ml)
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. customevaporated to dryness

출처 및 근거

ORD 기록
ord-fffbbb39f9e8456e96f6c75472942f70
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04791103

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