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

HRID 62071

反応式

HRID 62071 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-59d10e76a5ef44edbf2561405cf89fbe
出典データセット
uspto-grants-2016_09
特許番号
US09445594B2

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