Hydrochloric Acid → HCID 21931913、化合物

HRID 1453926ノート

反応式

HRID 1453926 の反応式
[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

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1133Thioglycolic AcidHCID 8000Boron trifluoride etherateHCID 11770077HCID 11770077、化合物

生成物 1

HCID 21931913HCID 21931913、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒2 回HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-7742bed10df5433ba131daa37775c7d0
出典データセット
uspto-grants-2009_01
特許番号
US07476690B2

反応ノート

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