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Sodium Bicarbonate → HCID 57475688、化合物

HRID 217994
ノート
印刷プレビュー

反応式

HRID 217994 の反応式
COCCN(S(F)(F)[F:11])CCOC.[N+:14]([C:17]1[CH:18]=[CH:19][C:20]([F:43])=[C:21]([C@@:23]23[N:32]=[C:31]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:39])([CH3:38])[CH3:37])[S:30][CH2:29][C@@H:28]2[CH2:27][C@H:26]([CH2:41]O)[O:25][CH2:24]3)[CH:22]=1)([O-:16])=[O:15].NC1C=CC(F)=C([C@@]23N=C(NC(=O)OC(C)(C)C)SC[C@@H]2[C@@H](OC)COC3)C=1.C(=O)(O)[O-].[Na+]>ClCCl>[N+:14]([C:17]1[CH:18]=[CH:19][C:20]([F:43])=[C:21]([C@@:23]23[N:32]=[C:31]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:38])([CH3:39])[CH3:37])[S:30][CH2:29][C@@H:28]2[CH2:27][C@H:26]([CH2:41][F:11])[O:25][CH2:24]3)[CH:22]=1)([O-:16])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 516892Sodium BicarbonateHCID 2734690(Bis(2-methoxyethyl)amino)sulfur trifluorideHCID 59281190HCID 59281190、化合物HCID 59281215HCID 59281215、化合物

生成物 1

HCID 57475688HCID 57475688、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

[Bis(2-methoxyethyl)amino]sulfur trifluoride (285 μl) was added dropwise to a solution of tert-butyl [(4aR,6R,8aS)-8a-(5-nitro-2-fluorophenyl)-6-hydroxymethyl-4,4a,5,6,8,8a-hexahydro-7-oxa-3-thia-1-azanaphthalen-2-yl]carbamate obtained in Preparation Example 13 (575 mg) in dichloromethane (55 ml) at −78° C. The mixture was stirred overnight with gradual heating to room temperature. A sodium bicarbonate solution was added to the reaction solution, and the aqueous layer was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by NH-silica gel column chromatography to obtain the title compound (240 mg).

後処理

  1. extractionthe aqueous layer was extracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by NH-silica gel column chromatography

出典と根拠

ORDレコード
ord-00a68af702d8415a982ae1234d161e41
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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