Ethyl Acetate → HCID 178473725、化合物

HRID 849425ノート

反応式

HRID 849425 の反応式
Cl.Cl.Cl.[NH:4]1[CH:8]=[C:7]([CH2:9][N:10]2[C:16]3[CH:17]=[CH:18][C:19]([C:21]4[CH:22]=N[CH:24]=[CH:25][CH:26]=4)=[CH:20][C:15]=3[CH2:14][N:13]([C:27](=[O:32])[C:28](F)(F)F)[CH:12]([CH2:33][C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:11]2)[N:6]=[CH:5]1.[Sn](Cl)[Cl:41].[C:43](OCC)(=O)C>>[ClH:41].[C:27]([N:13]1[CH2:14][C:15]2[CH:20]=[C:19]([C:21]3[CH:22]=[CH:43][CH:24]=[CH:25][CH:26]=3)[CH:18]=[CH:17][C:16]=2[N:10]([CH2:9][C:7]2[N:6]=[CH:5][NH:4][CH:8]=2)[CH2:11][C@H:12]1[CH2:33][C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1)(=[O:32])[CH3:28]

参加物

4

反応物 3

HCID 8857Ethyl AcetateHCID 24479Stannous ChlorideHCID 178478619HCID 178478619、化合物

生成物 1

HCID 178473725HCID 178473725、化合物収率 52%

実験手順

A mixture of Compound B (660 mg, 1.68 mmol), tin (II) chloride (1.52 g, 6.7 mmol) and ethyl acetate (75 mL) was stirred at room temperature for 18 hours and quenched with aqueous and then solid potassium carbonate (5 mL, then 5 gms). The mixture was filtered, the filtrate partitioned and the organic phase dried (MgSO4), concentrated in vacuum, and purified using flash chromatography (3:1 hexane:ethyl acetate) to provide Compound C (315 mg, 52%) as a clear oil.

後処理

  1. customquenched with aqueous and then solid potassium carbonate (5 mL
  2. filtrationThe mixture was filtered
  3. customthe filtrate partitioned
  4. dry with materialthe organic phase dried (MgSO4)
  5. concentrationconcentrated in vacuum
  6. custompurified

出典と根拠

ORDレコード
ord-68c0a6e5f2b94757874d08b924a83cff
出典データセット
uspto-grants-2000_01
特許番号
US06011029

反応ノート

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