Triethylamine → [1,1'-Biphenyl]-3-carbonyl azide

HRID 62071

반응식

HRID 62071 반응식
C1(P([N:15]=[N+:16]=[N-:17])(C2C=CC=CC=2)=O)C=CC=CC=1.C(N(CC)CC)C.[C:25]1([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:30]=[CH:29][CH:28]=[C:27]([C:31](O)=[O:32])[CH:26]=1>C(O)(C)C>[C:25]1([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([N:15]=[N+:16]=[N-:17])=[O:32])[CH:26]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12854(1,1'-Biphenyl)-3-carboxylic acidHCID 199401P,P-Diphenylphosphinic azide

생성물 1

HCID 118675061[1,1'-Biphenyl]-3-carbonyl azide수율 119.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a vial (8 mL) diphenylphosphoryl azide (0.39 mL, 1.8 mmol) and triethylamine (0.25 mL, 1.8 mmol) were added to a stirred solution of biphenyl-3-carboxylic acid (0.30 g, 1.5 mmol) in isopropanol (3 mL). The vial was closed with a lid, and the reaction mixture was stirred for 16 hours at room temperature. The reaction mixture was concentrated, and water (50 mL) was added. The mixture was extracted with ethyl acetate (3×50 mL). The combined extracts were dried over sodium sulfate, filtered, and concentrated to provide the title compound (0.40 g, 100%) was used in the next reaction without characterization or purification.

후처리

  1. customThe vial was closed with a lid
  2. concentrationThe reaction mixture was concentrated
  3. additionwater (50 mL) was added
  4. extractionThe mixture was extracted with ethyl acetate (3×50 mL)
  5. dry with materialThe combined extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-59d10e76a5ef44edbf2561405cf89fbe
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09445594B2

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