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Hydrochloric Acid → (3S)-piperidine-3-carboxylic acid hydrochloride

HRID 1771935
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HRID 1771935 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][C@H:10]([C:14]([OH:16])=[O:15])[CH2:9]1)=O)(C)(C)C.[ClH:17]>C(O)(=O)C>[ClH:17].[NH:8]1[CH2:13][CH2:12][CH2:11][C@H:10]([C:14]([OH:16])=[O:15])[CH2:9]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 6951168(3S)-1-((tert-butoxy)carbonyl)piperidine-3-carboxylic acid

생성물 1

HCID 24820453(3S)-piperidine-3-carboxylic acid hydrochloride수율 99.7%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
15 °C

실험 절차

(S)-Piperidine-1,3-dicarboxylic acid 1-tert-butyl ester (20 kg, 87.2 mol) was slurried in acetic acid (189 kg) and cooled to 15° C. An excess of hydrogen chloride gas (9.6 kg) was charged and stirred for ˜4 hours to complete deprotection. The slurry was isolated and filter-cake rinsed with acetic acid (2×31.5 kg). The filter cake was then vacuum dried to obtain product (14.4 kg).

후처리

  1. customThe slurry was isolated
  2. filtrationfilter-cake
  3. washrinsed with acetic acid (2×31.5 kg)
  4. customvacuum dried

출처 및 근거

ORD 기록
ord-925b7b092fbe451aa4d191be1ffa875b
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249155B2

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