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Hydrochloric Acid → (R)-2-methyl-4,4,4-trifluorobutylamine hydrochloride

HRID 327811
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HRID 327811 반응식
O.NN.[CH3:4][C@H:5]([CH2:18][C:19]([F:22])([F:21])[F:20])[CH2:6][N:7]1C(=O)C2C(=CC=CC=2)C1=O.[ClH:23]>C(O)C>[ClH:23].[CH3:4][C@H:5]([CH2:18][C:19]([F:22])([F:21])[F:20])[CH2:6][NH2:7]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 10378474(R)-2-(2-methyl-4,4,4-trifluorobutyl)-1H-isoindole-1,3(2H)-dione

생성물 1

HCID 12004108(R)-2-methyl-4,4,4-trifluorobutylamine hydrochloride수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Hydrazine monohydrate (3.1 mL) was added to a stirred solution of (R)-2-(2-methyl-4,4,4-trifluorobutyl)-1H-isoindole-1,3(2H)-dione (17.1 g) in anhydrous ethanol (85 mL) was heated to reflux. After three hours' reflux, the solution was cooled; ethanol (40 mL) was added; and the solution was acidified to pH 1 by addition of concentrated hydrochloric acid and was filtered. The filtrate was evaporated, and the residue was purified by sublimation (bath temperature 170° C., at 6.6 Pa) to yield (R)-2-methyl-4,4,4-trifluorobutylamine hydrochloride as a white solid (9.89 g, 88%); mp 187°-191° C.; partial NMR (300 MHz, DMSO-d6 -D2) shake): 1.05 (d,3H,CH3), 2.06-2.36(m,2H,CF3CH2) 2.36-2.54(m,1H,CHCH3) 2.73(dd,1H,CH2N), 2.87(dd,1H,CH2N) 8.20(br s,2H,NH2).

후처리

  1. temperaturewas heated to reflux
  2. temperatureAfter three hours' reflux
  3. temperaturethe solution was cooled
  4. filtrationwas filtered
  5. customThe filtrate was evaporated
  6. customthe residue was purified by sublimation (bath temperature 170° C., at 6.6 Pa)

출처 및 근거

ORD 기록
ord-0cf3da992e544b8096411774515f69df
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05274118

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