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Ammonium Chloride → HCID 59281186, 화합물

HRID 217993
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HRID 217993 반응식
[Cl-].[NH4+].[F:3][C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6][C:5]=1[C@@:13]12[N:22]=[C:21]([NH:23][C:24](=[O:30])[O:25][C:26]([CH3:29])([CH3:28])[CH3:27])[S:20][CH2:19][C@@H:18]1[CH2:17][C@H:16]([CH2:31][OH:32])[O:15][CH2:14]2>C(O)C.[Fe]>[NH2:10][C:7]1[CH:8]=[CH:9][C:4]([F:3])=[C:5]([C@@:13]23[N:22]=[C:21]([NH:23][C:24](=[O:30])[O:25][C:26]([CH3:28])([CH3:29])[CH3:27])[S:20][CH2:19][C@@H:18]2[CH2:17][C@H:16]([CH2:31][OH:32])[O:15][CH2:14]3)[CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 59281190HCID 59281190, 화합물

생성물 1

HCID 59281186HCID 59281186, 화합물수율 59.9%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매

실험 절차

Iron powder (121 mg) and a saturated ammonium chloride solution (1 ml) were added to a solution of tert-butyl [(4aR,6R,8aS)-8a-(2-fluoro-5-nitrophenyl)-6-hydroxymethyl-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate (120 mg) in ethanol (20 ml). The reaction solution was heated under reflux for 40 minutes and then cooled to room temperature. The insoluble matter was filtered off through celite, and the filtrate was evaporated under reduced pressure. The residue was purified by NH-silica gel column chromatography to obtain the title compound (67 mg).

후처리

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux for 40 minutes
  3. filtrationThe insoluble matter was filtered off through celite
  4. customthe filtrate was evaporated under reduced pressure
  5. customThe residue was purified by NH-silica gel column chromatography

출처 및 근거

ORD 기록
ord-789a8ca9c59e426d9f910963201502ee
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08198269B2

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