Diisopropylethylamine → N-(4-(Trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4-amine

HRID 2219964노트

반응식

HRID 2219964 반응식
ClC(OC(Cl)C)=O.C([N:15]1[CH2:24][CH2:23][C:22]2[C:21]([NH:25][C:26]3[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=3)=[N:20][C:19]([CH2:36][O:37][CH3:38])=[N:18][C:17]=2[CH2:16]1)C1C=CC=CC=1.C(N(C(C)C)CC)(C)C>ClCCCl>[F:35][C:32]([F:33])([F:34])[C:29]1[CH:30]=[CH:31][C:26]([NH:25][C:21]2[C:22]3[CH2:23][CH2:24][NH:15][CH2:16][C:17]=3[N:18]=[C:19]([CH2:36][O:37][CH3:38])[N:20]=2)=[CH:27][CH:28]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 5213051-Chloroethyl chloroformateHCID 120043937-Benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4-amine

생성물 1

HCID 59021578N-(4-(Trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4-amine

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
60 °C

실험 절차

1-Chloroethyl chloroformate (543 mg, 3.8 mmol) was added dropwise to the solution of 7-benzyl-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidin-4-amine from Example 31 (820 mg, 1.9 mmol) and diisopropylethyl amine (490 mg, 3.8 mmol) in 1,2-dichloroethane (5 mL, anhydrous) at room temperature. After addition, the reaction mixture was stirred at 60° C. for 2 h in the atmosphere of nitrogen. Solvent was removed in vacuo, residue was dissolved in methanol (10 mL) and was stirred at 60° C. for 1 hr. Solvent was removed in vacuo, residue was dissolved in ethyl acetate and was washed by sodium bicarbonate aqueous solution, brine and dried over sodium sulfate. Solvent was removed in vacuo and light orange oily residue was directly taken to the next step.

후처리

  1. additionAfter addition
  2. customSolvent was removed in vacuo, residue
  3. dissolutionwas dissolved in methanol (10 mL)
  4. stirringwas stirred at 60° C. for 1 hr
  5. customSolvent was removed in vacuo, residue
  6. dissolutionwas dissolved in ethyl acetate
  7. washwas washed by sodium bicarbonate aqueous solution, brine
  8. dry with materialdried over sodium sulfate
  9. customSolvent was removed in vacuo and light orange oily residue

출처 및 근거

ORD 기록
ord-f6e30175f127424789164b1090022f93
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07414131B2

반응 노트

불러오는 중…