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Thiobenzamide → Methyl 2-phenyl-4,5,6,7-tetrahydrobenzo[d]thiazole-7-carboxylate

HRID 1051917
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반응식

HRID 1051917 반응식
Br[CH:2]1[C:7](=O)[CH2:6][CH2:5][CH2:4][CH:3]1[C:9]([O:11][CH3:12])=[O:10].[C:13]([NH2:21])(=[S:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>CCO>[C:14]1([C:13]2[S:20][C:2]3[CH:3]([C:9]([O:11][CH3:12])=[O:10])[CH2:4][CH2:5][CH2:6][C:7]=3[N:21]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 683563ThiobenzamideHCID 83646766HCID 83646766, 화합물

생성물 1

HCID 90303482Methyl 2-phenyl-4,5,6,7-tetrahydrobenzo[d]thiazole-7-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A soln. of methyl 2-bromo-3-oxocyclohexanecarboxylate (100 mg, 0.43 mmol) and thiobenzamide (64 mg, 0.47 mmol) in EtOH (2 mL) was stirred at 85° C. overnight. Subsequently, the mixture was quenched with aq. sat. NaHCO3 and extracted with EtOAc. The comb. org. layers were washed with brine, dried over MgSO4, and conc. in vacuo. Purification by means of CC (2-15% EtOAc/Hept) provided a yellow oil.

후처리

  1. customSubsequently, the mixture was quenched with aq. sat. NaHCO3
  2. extractionextracted with EtOAc
  3. washlayers were washed with brine
  4. dry with materialdried over MgSO4
  5. customPurification by means of CC (2-15% EtOAc/Hept)
  6. customprovided a yellow oil

출처 및 근거

ORD 기록
ord-6e769148e7034c299eae2b771e341106
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09388197B2

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