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Benzenesulfonyl chloride → Hydrazinecarboxylic acid, 2-(phenylsulfonyl)-, methyl ester

HRID 596926
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HRID 596926 반응식
[C:1]([O:5][CH3:6])(=[O:4])[NH:2][NH2:3].C(=O)(O)[O-].[Na+].[C:12]1([S:18](Cl)(=[O:20])=[O:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>O>[C:12]1([S:18]([NH:3][NH:2][C:1]([O:5][CH3:6])=[O:4])(=[O:20])=[O:19])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7369Benzenesulfonyl chlorideHCID 80519Methyl carbazateHCID 516892Sodium Bicarbonate

생성물 1

HCID 8501001Hydrazinecarboxylic acid, 2-(phenylsulfonyl)-, methyl ester

시약·촉매·용매 1

HCID 962Water용매

실험 절차

180 g. (0.2 mole) of methyl carbazate (from hydrazine and dimethyl carbonate) is placed in a liter flask. 20.0 g. (0.24 mole) of sodium bicarbonate and 100 ml. water are added. The mixture is stirred and dropped in 35.2 g. (0.2 mole) of benzene sulfonyl chloride. Then the mixture is stirred for 16 hours. The crystals that have formed are filtered off, washed with water, and dried in air. Yield = 34.5 g.; m.p. 149°-154° C. Upon recrystallization from ethanol 26 g. of material is recovered which melts sharply at 155° C.

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후처리

  1. additiondropped in 35.2 g
  2. stirringThen the mixture is stirred for 16 hours
  3. customThe crystals that have formed
  4. filtrationare filtered off
  5. washwashed with water
  6. customdried in air
  7. customUpon recrystallization from ethanol 26 g
  8. customof material is recovered which melts sharply at 155° C.

출처 및 근거

ORD 기록
ord-1858ef5995844c61bd709e1ae8ad3f5f
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04012432

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