Hydrochloric Acid → HCID 69885803, 화합물

HRID 1280620노트

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HRID 1280620 반응식
C([NH:5][C:6]([NH:8][C@H:9]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:10]O)=[S:7])(C)(C)C.[ClH:19]>C(OCC)C>[ClH:19].[C:13]1([CH2:12][C@@H:9]2[CH2:10][S:7][C:6]([NH2:5])=[N:8]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 86584424N-(tert-butyl)-N'-[(1R)-2-hydroxy-1-(phenylmethyl)ethyl]thiourea

생성물 1

HCID 69885803HCID 69885803, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

The process is performed as in Example 2, starting with 2 g of N-(tert-butyl)-N′-[(1R)-2-hydroxy-1-(phenylmethyl)ethyl]thiourea and 20 cm3 of aqueous 6N hydrochloric acid. The reaction lasts 1 h 30 min. After cooling the reaction mass to a temperature in the region of 0° C., the solution is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. Crystallization of the oil obtained is initiated by addition of diethyl ether. The resulting precipitate is spin-filtered, washed with twice 10 cm3 of diethyl ether and then dried under reduced pressure (10 Pa) at a temperature in the region of 60° C. The product is purified by taking it up in 100 cm3 of dichloromethane with stirring for 30 minutes. After filtration of the suspension, the filter cake is washed with twice 10 cm3 of dichloromethane and is then dried under the same conditions as above. 1.1 g of (+)-(4R)-4-phenylmethyl-4,5-dihydro-1,3-thiazol-2-ylamine hydrochloride are obtained in the form of a white solid melting at 168° C. (αD2032 +8.7±0.3 at a concentration of 1% in methanol).

후처리

  1. concentrationthe solution is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C
  2. customCrystallization of the oil
  3. customobtained
  4. filtrationThe resulting precipitate is spin-filtered
  5. washwashed with twice 10 cm3 of diethyl ether
  6. customdried under reduced pressure (10 Pa) at a temperature in the region of 60° C
  7. customThe product is purified
  8. filtrationAfter filtration of the suspension
  9. washthe filter cake is washed with twice 10 cm3 of dichloromethane
  10. customis then dried under the same conditions as above

출처 및 근거

ORD 기록
ord-99a28f861f6c4ac59705a12c91ed114b
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451821B1

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