Ethyl Acetate → HCID 178473725, 화합물

HRID 849425노트

반응식

HRID 849425 반응식
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]

참가 물질

4

반응물 3

HCID 8857Ethyl AcetateHCID 24479Stannous ChlorideHCID 178478619HCID 178478619, 화합물

생성물 1

HCID 178473725HCID 178473725, 화합물수율 52%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-68c0a6e5f2b94757874d08b924a83cff
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06011029

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