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Ammonium Chloride → HCID 59281186、化合物

HRID 217993
ノート
印刷プレビュー

反応式

HRID 217993 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 59281190HCID 59281190、化合物

生成物 1

HCID 59281186HCID 59281186、化合物収率 59.9%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-789a8ca9c59e426d9f910963201502ee
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08198269B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート