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Potassium Phosphate, Tribasic → Ethyl 3-chloro-5-(4-methylcyclohex-1-en-1-yl)-1,2-thiazole-4-carboxylate

HRID 2177404
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HRID 2177404 반응식
[Cl:1][C:2]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:5](Cl)[S:4][N:3]=1.[CH3:13][CH:14]1[CH2:19][CH2:18][C:17](B(O)O)=[CH:16][CH2:15]1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O1CCOCC1>[Cl:1][C:2]1[C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:5]([C:17]2[CH2:18][CH2:19][CH:14]([CH3:13])[CH2:15][CH:16]=2)[S:4][N:3]=1
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참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 441195564-Methylcyclohexen-1-ylboronic acidHCID 90418456Ethyl 3,5-dichloro-1,2-thiazole-4-carboxylate

생성물 1

HCID 118184949Ethyl 3-chloro-5-(4-methylcyclohex-1-en-1-yl)-1,2-thiazole-4-carboxylate수율 63.6%

시약·촉매·용매 2

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

Into a 25-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen was placed ethyl 3,5-dichloro-1,2-thiazole-4-carboxylate (150 mg, 0.66 mmol, 1.00 equiv), (4-methylcyclohex-1-en-1-yl)boronic acid (103 mg, 0.74 mmol, 1.11 equiv), Pd(PPh3)4 (38 mg, 0.03 mmol, 0.05 equiv), K3PO4 (368 mg, 1.73 mmol, 2.61 equiv), dioxane (3 mL). The resulting solution was stirred overnight at 90° C. in an oil bath. The solids were removed by filtration. The resulting mixture was concentrated under reduced pressure. The residue was applied to a silica gel column, eluting with ethyl acetate/petroleum ether (2:98) to afford 120 mg (63%) of ethyl 3-chloro-5-(4-methylcyclohex-1-en-1-yl)-1,2-thiazole-4-carboxylate as a colorless oil.

후처리

  1. customInto a 25-mL round-bottom flask purged
  2. temperaturemaintained with an inert atmosphere of nitrogen
  3. customThe solids were removed by filtration
  4. concentrationThe resulting mixture was concentrated under reduced pressure
  5. washeluting with ethyl acetate/petroleum ether (2:98)

출처 및 근거

ORD 기록
ord-0aebdce638564bde939d34ba08dd6a63
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067898B1

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