tert-Butanol → N,N-diethyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4-amine

HRID 22787

반응식

HRID 22787 반응식
Cl[C:2]1[C:3]2[C:10]3[CH2:11][CH2:12][CH2:13][C:9]=3[S:8][C:4]=2[N:5]=[CH:6][N:7]=1.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15].[C:19](O)(C)(C)C.CCOC(C)=O>O.Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:2]1[C:3]2[C:10]3[CH2:19][CH2:11][CH2:12][CH2:13][C:9]=3[S:8][C:4]=2[N:5]=[CH:6][N:7]=1)[CH3:15]

참가 물질

6

반응물 4

HCID 6386tert-ButanolHCID 8021Diethylamine2회HCID 8857Ethyl AcetateHCID 78981712-Chloro-7-thia-9,11-diazatricyclo(6.4.0.0,2,6)dodeca-1(12),2(6),8,10-tetraene

생성물 1

HCID 717848N,N-diethyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4-amine

시약·촉매·용매 1

HCID 21885828Hydrate;hydrochloride용매

실험 절차

To a slurry of 0.044 g 4-chloro-6,7-dihydro-5H-cyclopenta[4,5]thieno[2,3-d]pyrimidine (0.196 mmol) in 1 mL of 100:1 H2O/HCl was added 0.014 g (0.02 mL, 0.106 mmol) diethylamine. The mixture was heated to reflux, and an additional 0.2 mL diethylamine and 1 mL of t-butanol were added and heated continued at reflux for an additional 1 h. TLC (20% EtOAc/80% pet ether) showed complete reaction and the 1H NMR of the isolated material was consistent with the desired product.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureheated
  4. temperatureat reflux for an additional 1 h
  5. customreaction

출처 및 근거

ORD 기록
ord-dcfb3b429c2544d6bb6f40646bccd630
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849638B2

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