Water → HCID 9932026, 화합물

HRID 2292494노트

반응식

HRID 2292494 반응식
Cl([O-])=O.[Na+].[F:5][C:6]1[CH:34]=[CH:33][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([CH:31]=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:8][CH:7]=1.P([O-])([O-])([O-])=[O:36].[Na+].[Na+].[Na+].O>CC(=CC)C.C1COCC1.C(O)(=O)C.C(O)(C)(C)C>[F:5][C:6]1[CH:7]=[CH:8][C:9]([C:10]([C@H:12]2[CH2:17][CH2:16][C@H:15]3[C@H:18]4[C@H:28]([CH2:29][CH2:30][C@:13]23[CH3:14])[C@:26]2([CH3:27])[C:21]([CH:22]=[C:23]([C:31]([OH:36])=[O:32])[CH2:24][CH2:25]2)=[CH:20][CH2:19]4)=[O:11])=[CH:33][CH:34]=1

참가 물질

9

반응물 4

HCID 962WaterHCID 24243Trisodium PhosphateHCID 23668197Sodium ChloriteHCID 54571409HCID 54571409, 화합물

생성물 1

HCID 9932026HCID 9932026, 화합물

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 6386tert-Butanol용매HCID 8028Tetrahydrofuran용매HCID 105532-Methyl-2-butene용매

실험 절차

Sodium chlorite is added to a mixture of 17β-(4-fluorobenzoyl)-androsta-3,5-diene-3-carboxaldehyde, sodium phosphate, monobasic monohydrate in 2-methyl-2-butene in THF, H2O, and t-butanol at RT. After 6 h acetic acid was added, then the aqueous layer is extracted with EtOAc, the combined organic extracts are dried (MgSO4), filtered, concentrated, and flash chromatographed to yield the title compound.

후처리

  1. customat RT
  2. extractionthe aqueous layer is extracted with EtOAc
  3. dry with materialthe combined organic extracts are dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customflash chromatographed

출처 및 근거

ORD 기록
ord-b2c1cb349a34487c93452157e22a20ca
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05683995

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