Triethylamine → HCID 18997000、化合物

HRID 374648ノート

反応式

HRID 374648 の反応式
[CH3:1][O:2][C:3]1[C:16]2[C:15](=[O:17])[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][C:13]=3[O:18][CH3:19])[C:8](=[O:20])[C:7]=2[CH:6]=[C:5]([C:21]([OH:23])=O)[CH:4]=1.C(N(CC)CC)C.C1(P([N:45]=[N+:46]=[N-:47])(C2C=CC=CC=2)=O)C=CC=CC=1>CN(C=O)C>[CH3:1][O:2][C:3]1[C:16]2[C:15](=[O:17])[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][C:13]=3[O:18][CH3:19])[C:8](=[O:20])[C:7]=2[CH:6]=[C:5]([C:21]([N:45]=[N+:46]=[N-:47])=[O:23])[CH:4]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 99727772-Anthracenecarboxylic acid, 9,10-dihydro-4,5-dimethoxy-9,10-dioxo-

生成物 1

HCID 18997000HCID 18997000、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

9,10-Dihydro-4,5-dimethoxy-9,10-dioxoanthracene-2-carboxylic acid (10 g) was suspended in dry DMF (130 ml) and cooled to 0° C. Triethylamine (3.89 g) was then carefully added, followed by a solution of diphenylphosphoryl azide (10.57 g) in dry DMF (20 ml). A yellow precipitate was generated during 12 hours stirring at room temperature. The precipitate was collected by filtration and washed with saturated sodium bicarbonate solution (1×100 ml) and water (5×100 ml). Drying in vacuo over silica gel yielded 9,10-dihydro-4,5-dimethoxy-9,10-dioxoanthracene-2-carbonyl azide as a signal yellow powder. Decomposition point: 139° C.

後処理

  1. filtrationThe precipitate was collected by filtration
  2. washwashed with saturated sodium bicarbonate solution (1×100 ml) and water (5×100 ml)
  3. customDrying in vacuo over silica gel

出典と根拠

ORDレコード
ord-ec77fbc495d844879e0dbdab7557b94b
出典データセット
uspto-grants-1996_01
特許番号
US05480873

反応ノート

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