Sodium Iodide → HCID 178446918, 화합물

HRID 1252229노트

반응식

HRID 1252229 반응식
Cl[CH2:2][C:3]([CH3:8])([CH3:7])[C:4]([O-])=[O:5].[Na+].ClCC(C)(C)C(O)=O.[H-].[Na+].C[Si](C)(C)Cl.[C:25]([O-:33])(=S)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.[Na+].C(O)(=[S:42])C1C=CC=CC=1.[I-].[Na+]>CN(C)C=O>[C:25]([CH2:2][C:3]([CH3:8])([CH3:7])[C:4]([OH:5])=[S:42])(=[O:33])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

9

반응물 7

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 24758Sodium hydride2회HCID 83542beta-Chloropivalic acidHCID 23670066Sodium beta-chloropivalateHCID 23688990Benzenecarbothioic acid, sodium salt (1:1)HCID 178526132HCID 178526132, 화합물

생성물 1

HCID 178446918HCID 178446918, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매3회

실험 절차

To a solution of sodium β-chloropivalate, prepared from β-chloropivalic acid (13.66 g) and 50% sodium hydride (4.80 g) in dimethylformamide (110 ml) was added dropwise trimethyl chlorosilane (10.85 g) in dimethylformamide (10 ml) at -5° C. to -3° C. After stirring for 1 hour sodium thiobenzoate, prepared from thiobenzoic acid (13.8 g) and 50% sodium hydride (4.80 g) in dimethylformamide (70 ml), was added dropwise thereto at -5° C. to -8° C. After addition of sodium iodide (15.0 g), the mixture was stirred at room temperature for 3 days and then at 40° C. for 7 days. The reaction mixture was diluted with ice-water and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous sodium sulfate and evaporated in vacuo. The residue was recrystallized from diisopropyl ether-petroleum ether to give β-benzoylthiopivalic acid.

후처리

  1. additionwas added dropwise
  2. customat -5° C. to -8° C
  3. waitat 40° C. for 7 days
  4. extractionextracted with ethyl acetate
  5. extractionThe ethyl acetate extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated in vacuo
  9. customThe residue was recrystallized from diisopropyl ether-petroleum ether

출처 및 근거

ORD 기록
ord-a73e3a68e2864043b4a93df3f09debc4
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742052

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