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Acetonitrile → 4-[4-(2,5-Dichlorobenzoyl)phenoxy]benzene-1-sulfonyl chloride

HRID 2246027
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인쇄 미리보기

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HRID 2246027 반응식
C(#N)C.S1(CCCC1)(=O)=O.[Na+].[Cl:12][C:13]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:14]=1[C:15]([C:17]1[CH:33]=[CH:32][C:20]([O:21][C:22]2[CH:27]=[CH:26][C:25]([S:28]([O-])(=[O:30])=[O:29])=[CH:24][CH:23]=2)=[CH:19][CH:18]=1)=[O:16].P(Cl)(Cl)([Cl:41])=O>O.CN(C)C(=O)C>[Cl:12][C:13]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:14]=1[C:15]([C:17]1[CH:33]=[CH:32][C:20]([O:21][C:22]2[CH:27]=[CH:26][C:25]([S:28]([Cl:41])(=[O:30])=[O:29])=[CH:24][CH:23]=2)=[CH:19][CH:18]=1)=[O:16]
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참가 물질

7

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HCID 6342AcetonitrileHCID 24813Phosphorus oxychlorideHCID 31347SulfolaneHCID 237098054-[4-(2,5-Dichlorobenzoyl)phenoxy]benzene sulfonic acid sodium salt

생성물 1

HCID 179652914-[4-(2,5-Dichlorobenzoyl)phenoxy]benzene-1-sulfonyl chloride

시약·촉매·용매 2

HCID 962
Water
용매
HCID 31374Dimethylacetamide용매

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온도
72 °C

실험 절차

Solvent (300 mL of acetonitrile and 200 mL of sulfolane) was added to 215 g (about 400 mmol) of crude crystal of A—SO3Na. Furthermore, phosphoryl trichloride (245.3 g, 1.6 mol) was added and reacted at 70° C. Furthermore, 5 mL of N,N-dimethylacetamide was added, a yellow suspension was stirred for 40 minutes at 71 to 73° C., and the reaction liquid was cooled to 3° C. 1 L of cold water was added at a rate so that the temperature of the reaction liquid did not exceed 10° C. The deposit was filtered and collected, washed with cold water, and recrystallized with 350 mL of toluene to obtain 153 of white crystal of 4-[4-(2,5-dichlorobenzoyl)phenoxy]benzene sulfonic acid chloride (A—SO3Cl). Yield depending on A was 87%. Melting point is 130.5 to 131.5° C.

후처리

  1. customreacted at 70° C
  2. customthe reaction liquid
  3. temperaturewas cooled to 3° C
  4. customdid not exceed 10° C
  5. filtrationThe deposit was filtered
  6. customcollected
  7. washwashed with cold water
  8. customrecrystallized with 350 mL of toluene

출처 및 근거

ORD 기록
ord-ae7d72329dc54d0db9bd68fd2f453437
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07687187B2

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