Hydrochloric Acid → HCID 21931913, 화합물

HRID 1453926노트

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HRID 1453926 반응식
[C:1]1([C:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]=2[CH2:16]O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18]([OH:22])(=[O:21])[CH2:19][SH:20].B(F)(F)F.[CH3:27][CH2:28]OCC.Cl>ClCCCl.O>[C:1]1([C:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]=2[CH2:16][S:20][CH2:19][C:18]([O:22][CH2:27][CH3:28])=[O:21])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1133Thioglycolic AcidHCID 8000Boron trifluoride etherateHCID 11770077HCID 11770077, 화합물

생성물 1

HCID 21931913HCID 21931913, 화합물

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매2회HCID 962Water용매

실험 절차

A 250 mL round-bottom flask containing a magnetic stirring bar equipped with a reflux condenser was charged with 1.6 g (0.00717 mol) of compound 62, 0.8 mL (0.00717 mol) of thioglycolic acid and 50 mL of 1,2-dichloroethane. At 0° C., 1.4 mL (0.0107 mol) of BF3.Et2O dissolved in 10 mL of 1,2-dichloroethane was added slowly. The resulting mixture was stirred for 15 minutes and then 100 mL of water and 10 mL of HCl (1N) were added. The product was extracted with 2×50 mL of ethyl acetate. The organic layer was dried over magnesium sulfate, filtered and evaporated to dryness. The crude product was used for the next step (preparation of Example 148).

후처리

  1. additionA 250 mL round-bottom flask containing a magnetic stirring bar
  2. customequipped with a reflux condenser
  3. additionwas added slowly
  4. extractionThe product was extracted with 2×50 mL of ethyl acetate
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customThe crude product was used for the next step (preparation of Example 148)

출처 및 근거

ORD 기록
ord-7742bed10df5433ba131daa37775c7d0
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07476690B2

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