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Hydrochloric Acid → HCID 117778748, 화합물

HRID 2201762
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HRID 2201762 반응식
Cl.C([NH:9][C@@H:10]([C@@H:44]1[C@H:48]([CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH3:62])[O:47]C(C)(C)[O:45]1)[CH2:11][O:12][C@H:13]1[C@H:19]([O:20]CC2C=CC=CC=2)[C@@H:18]([O:28]CC2C=CC=CC=2)[C@@H:17]([O:36]CC2C=CC=CC=2)[CH:16]=[CH:15][CH2:14]1)C1C=CC=CC=1.C1CCCCC=1>CO.C(Cl)(Cl)Cl.[Pd]>[NH2:9][C@@H:10]([C@@H:44]([OH:45])[C@@H:48]([OH:47])[CH2:49][CH2:50][CH2:51][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH3:62])[CH2:11][O:12][C@@H:13]1[CH2:14][CH2:15][CH2:16][C@H:17]([OH:36])[C@H:18]([OH:28])[C@H:19]1[OH:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 8079CyclohexeneHCID 117778423HCID 117778423, 화합물

생성물 1

HCID 117778748HCID 117778748, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매
HCID 6212
Chloroform
용매

실험 절차

A 1M solution of HCl (150 μL, 0.15 mmol) and Pd—C (10% wt, 32 mg, 0.03 mmol) were added to a solution of ether 71 (130 mg, 0.15 mmol) and cyclohexene (2 mL) in MeOH (10 mL) and heated under reflux. After stirring overnight the reaction mixture was cooled to rt and diluted with a 5:1 solution of CHCl3:MeOH, before being filtered thought a bed of celite. The filtrate was concentrated under reduced pressure to provide the crude amine 72, which was used directly in the next step.

후처리

  1. temperatureheated
  2. temperatureunder reflux
  3. filtrationMeOH, before being filtered
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d37810fb4e1c478c84a1293cc42b767c
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365496B2

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