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Hydrochloric Acid → HCID 57386562、化合物

HRID 420268
ノート
印刷プレビュー

反応式

HRID 420268 の反応式
Cl.[NH2:2][C@@H:3]1[C@@H:8]([OH:9])[C@H:7]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([F:20])[CH:12]=2)[CH2:6][S:5](=[O:22])(=[O:21])[CH2:4]1.CC([O-])=O.[Na+].[C:28]([C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][CH:39]=1)[CH:35]=O)([CH3:31])([CH3:30])[CH3:29].[BH3-]C#N.[Na+].Cl.C([O-])([O-])=O.[K+].[K+]>CO.C(Cl)Cl>[C:28]([C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][CH:39]=1)[CH2:35][NH:2][C@@H:3]1[C@@H:8]([OH:9])[C@H:7]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[C:13]([F:20])[CH:12]=2)[CH2:6][S:5](=[O:22])(=[O:21])[CH2:4]1)([CH3:31])([CH3:29])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 517045Sodium AcetateHCID 5003444Sodium cyanoborohydrideHCID 101925883-Tert-butylbenzaldehydeHCID 131729360HCID 131729360、化合物

生成物 1

HCID 57386562
HCID 57386562、化合物

試薬・触媒・溶媒 1

HCID 21226129Dichloromethane methanol溶媒

実験手順

To a solution of (3R*,4S*,5S*)-3-amino-5-(3-fluoro-4-nitro-benzyl)-1,1-dioxo-hexahydro-1lambda*6*-thiopyran-4-ol hydrochloride (0.14 g, 0.39 mmol) in MeOH-CH2Cl2 1:1 (3 mL) was added NaOAc (0.065 g, 0.78 mmol) and 3-tert-butyl-benzaldehyde (0.07 g, 0.43 mmol). The reaction mixture was stirred at 25° C. for 0.5 h before NaBH3CN (0.039 g, 0.59 mmol) was added followed by stirring for 16 h. The reaction mixture was acidified with 1N aq. HCl, stirred for 15 min, basified with K2CO3-solution and extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4 and evaporated. The title compound was obtained after purification by flash-chromatography on silica gel (hexane-CH2Cl2-MeOH 20:20:1 to 1:20:5) as a light yellow foam: TLC (EtOAc) Rf=0.45; HPLC RtA=1.78 min; ESIMS [M+H]+=465; 1H NMR (400 MHz, CDCl3): δ 8.02 (t, 1H), 7.1-7.4 (m, 6H), 4.18 (s, 1H), 3.88 (d, 1H), 3.78 (d, 1H), 3.64 (m, 1H), 3.41 (ddd, 1H), 3.24 (ddd, 1H), 3.12 (dt, 1H), 3.00 (dd, 1H), 2.84, (m, 2H), 2.69 (m, 2H), 2.44 (m, 1H), 1.33 (s, 9H).

後処理

  1. additionwas added
  2. stirringstirred for 15 min
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. customevaporated

出典と根拠

ORDレコード
ord-175a6f05e00d4d73b710c74cd49283eb
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093406B2

反応ノート

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