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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetonitrile → Benzenesulfonyl chloride, 4-chloro-3-nitro-

HRID 1588380
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HRID 1588380 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([O-])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[K+].C(#N)C.CC(N(C)C)=O.P(Cl)(Cl)([Cl:27])=O>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([Cl:27])(=[O:10])=[O:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]
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참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 24813Phosphorus oxychlorideHCID 31374DimethylacetamideHCID 81181Benzenesulfonic acid, 4-chloro-3-nitro-, potassium salt

생성물 1

HCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-수율 84%

시약·촉매·용매 1

HCID 962Water
용매
2회

실험 절차

To a mixture of 1280 g of potassium 4-chloro-3-nitrobenzenesulfonate, 1150 ml of acetonitrile, 250 ml of sulforan, and 30 ml of dimethylacetamide was added dropwise 1250 ml of phosphorus oxychloride while maintaining the internal temperature thereof at 60° C. to 70° C. Then, after performing reaction for 3 hours at 73° C., the reaction mixture was cooled with water and after gradually adding thereto 400 ml of water, the reaction mixture was poured into 5 liters of ice-water. Crystals deposited were filtered by filtration, washed with water, and then dried to provide 1060 g of the above-described product with a yield of 84%. The melting point thereof was 55° C. to 56° C.

후처리

  1. temperaturewhile maintaining the internal temperature
  2. customat 60° C. to 70° C
  3. customreaction for 3 hours at 73° C.
  4. additionafter gradually adding
  5. filtrationCrystals deposited were filtered by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-e0defde8f7604cc6af9fbc0011caef44
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05221750

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