Hydrochloric Acid → Pevonedistat Hydrochloride

HRID 715631노트

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HRID 715631 반응식
[S:1](=[O:31])(=[O:30])([O:3][CH2:4][C@@H:5]1[CH2:9][C@@H:8]([N:10]2[C:14]3[N:15]=[CH:16][N:17]=[C:18]([NH:19][C@@H:20]4[C:28]5[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=5)[CH2:22][CH2:21]4)[C:13]=3[CH:12]=[CH:11]2)[CH2:7][C@@H:6]1[OH:29])[NH2:2].[ClH:32]>C(O)C>[ClH:32].[S:1](=[O:31])(=[O:30])([O:3][CH2:4][C@@H:5]1[CH2:9][C@@H:8]([N:10]2[C:14]3[N:15]=[CH:16][N:17]=[C:18]([NH:19][C@@H:20]4[C:28]5[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=5)[CH2:22][CH2:21]4)[C:13]=3[CH:12]=[CH:11]2)[CH2:7][C@@H:6]1[OH:29])[NH2:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 16720766Pevonedistat

생성물 1

HCID 66576990Pevonedistat Hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
22.5 °C

실험 절차

To a reaction vessel is added ((1S,2S,4R)-4-{4-[(1S)-2,3-dihydro-1H-inden-1-ylamino]-7H-pyrrolo[2,3-d]pyrimidin-7-yl}-2-hydroxycyclopentyl)methyl sulfamate (1 equiv.) and ethanol (15 volumes with respect to input material) and the mixture is stirred at 20-25° C. 1.0M hydrogen chloride in ethanol (1 equiv. with respect to input material) is added at a rate as to maintain temperature at ≦25° C. The mixture is then stirred at 20±5° C. for a minimum of 4 hours. The solid product is isolated by filtration and washed with ethanol (2×2.5 volumes with respect to input material). The product is then dried by aspiration on the filter and then under reduced pressure at a temperature of 30±5° C. to give the title compound.

후처리

  1. temperatureto maintain temperature at ≦25° C
  2. stirringThe mixture is then stirred at 20±5° C. for a minimum of 4 hours
  3. customThe solid product is isolated by filtration
  4. washwashed with ethanol (2×2.5 volumes with respect to input material)
  5. customThe product is then dried by aspiration on the
  6. filtrationfilter

출처 및 근거

ORD 기록
ord-f808676ce36a4c099d648f5f3a3bbe76
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187482B2

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