Aluminum(III) Chloride → HCID 58181130, 화합물

HRID 469315노트

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HRID 469315 반응식
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8](Cl)=[O:9])[CH:3]=1.[CH3:11][C:12]1[C:17]2[NH:18][C:19](=[O:21])[S:20][C:16]=2[CH:15]=[CH:14][CH:13]=1.[Cl-].[Cl-].[Cl-].[Al+3]>CCOC(C)=O>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([C:8]([C:14]2[CH:13]=[C:12]([CH3:11])[C:17]3[NH:18][C:19](=[O:21])[S:20][C:16]=3[CH:15]=2)=[O:9])[CH:3]=1

참가 물질

5

반응물 3

HCID 6451240Aluminum(III) ChlorideHCID 127708804-Methylbenzo[d]thiazol-2-olHCID 184220986-Chloropyrimidine-4-carbonyl chloride

생성물 1

HCID 58181130HCID 58181130, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
130 °C

실험 절차

1.93 g (10.0 mmol) 6-chloropyrimidine-4-carboxylic acid chloride, 1.80 g (10.9 mmol) 4-methyl-3H-benzothiazol-2-one and 7.33 g (55.0 mmol) aluminium trichloride were combined and heated to 130° C. for 3 h with stirring. The mixture was combined with ice water and EtOAc, the flakes formed were suction filtered and the phases were separated. The aqueous phase was extracted with EtOAc. The organic phases were combined, dried on sodium sulphate, filtered and the filtrate was evaporated down i. vac. The residue was triturated with DIPE, the precipitate was suction filtered and dried.

후처리

  1. customthe flakes formed
  2. filtrationwere suction filtered
  3. customthe phases were separated
  4. extractionThe aqueous phase was extracted with EtOAc
  5. customdried on sodium sulphate
  6. filtrationfiltered
  7. customthe filtrate was evaporated down i
  8. customThe residue was triturated with DIPE
  9. filtrationfiltered
  10. customdried

출처 및 근거

ORD 기록
ord-b829636732e74a968a4f9823bae57d14
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629137B2

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