Triethylamine → HCID 13772850, 화합물

HRID 978572노트

반응식

HRID 978572 반응식
[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[N:8]2[CH2:11][CH:10]([C:12]([OH:14])=O)[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N1C=CN=C1)([N:23]1[CH:27]=[CH:26]N=C1)=O.C(N(CC)CC)C.Cl.C(N)C>C(#N)C>[C:1]1([CH:7]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[N:8]2[CH2:9][CH:10]([C:12]([NH:23][CH2:27][CH3:26])=[O:14])[CH2:11]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11198Ethylamine hydrochlorideHCID 682631,1'-CarbonyldiimidazoleHCID 27354401-(Diphenylmethyl)azetidine-3-carboxylic acid

생성물 1

HCID 13772850HCID 13772850, 화합물수율 114%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
60 °C

실험 절차

To a solution of 7.5 g (28 mmole) of 1-(diphenylmethyl)azetidine-3-carboxylic acid in 75 ml of acetonitrile was added 6.0 g (37 mmole) of 1,1'-carbonyldiimidazole. The reaction was heated at 60° C. for two hours and successively treated with 3.1 g (30.8 mmole) of triethylamine and 2.52 g (30.8 mmole) of ethylamine hydrochloride. The reaction was stirred at 60° C. for an additional hour, the solvent evaporated in vacuo and the residue dissolved in chloroform. After washing with water and drying over magnesium sulfate, the chloroform layer was evaporated in vacuo to give 9.4 g of 1-(diphenylmethyl)-N-ethyl-3-azetidinecarboxamide, mp 91°-93° C.

후처리

  1. customthe solvent evaporated in vacuo
  2. dissolutionthe residue dissolved in chloroform
  3. washAfter washing with water
  4. dry with materialdrying over magnesium sulfate
  5. customthe chloroform layer was evaporated in vacuo

출처 및 근거

ORD 기록
ord-174a8d57ad9b4d3fa1931db8287d8fbd
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04665079

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