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Hydrochloric Acid → Pruvanserin hydrochloride

HRID 1013056
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HRID 1013056 반응식
[CH2:1]1[N:6]([CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2F)[CH2:5][CH2:4][N:3]([C:17]([C:19]2[C:24]3[NH:25][CH:26]=[C:27]([C:28]#[N:29])[C:23]=3[CH:22]=[CH:21][CH:20]=2)=[O:18])[CH2:2]1.O.[ClH:31]>CC(C)=O>[ClH:31].[F:15][C:12]1[CH:13]=[CH:14][C:9]([CH2:8][CH2:7][N:6]2[CH2:5][CH2:4][N:3]([C:17]([C:19]3[CH:20]=[CH:21][CH:22]=[C:23]4[C:24]=3[NH:25][CH:26]=[C:27]4[C:28]#[N:29])=[O:18])[CH2:2][CH2:1]2)=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 220175507-(1-(2,4-difluorophenethyl)piperazine-4-carbonyl)-1H-indole-3-carbonitrile

생성물 1

HCID 9887933Pruvanserin hydrochloride수율 69%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

2.1 g of the free base of EMD281014 are heated in 50 ml of acetone, and water is added until a clear solution is formed. A mixture of 0.6 ml of hydrochloric acid (w=37%) and 1.2 ml of acetone is then stirred in. The mixture is subsequently evaporated to half the volume in a rotary evaporator. The precipitated hydrochloride is filtered off with suction, washed with acetone and diethyl ether and dried, giving 1.6 g of 7-{4-[2-(4-fluorophenyl)ethyl]-piperazine-1-carbonyl}-1H-indole-3-carbonitrile, hydrochloride (69% of theory), decomposition range 314-319°.

후처리

  1. customis formed
  2. customThe mixture is subsequently evaporated to half the volume
  3. customin a rotary evaporator
  4. filtrationThe precipitated hydrochloride is filtered off with suction
  5. washwashed with acetone and diethyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-2ca00d1822e0467c964b916007dd649f
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981897B2

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