Ammonia → HCID 14650455、化合物

HRID 1200187ノート

反応式

HRID 1200187 の反応式
[C:1]1([C:7]2[O:8][C:9]3[C:17]([CH2:18][C:19]([OH:21])=O)=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1.C([N:24](CC)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1.N>CCCCCC.ClCCl>[C:1]1([C:7]2[O:8][C:9]3[C:17]([CH2:18][C:19]([NH2:24])=[O:21])=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1

参加物

7

反応物 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 14650449HCID 14650449、化合物

生成物 1

HCID 14650455HCID 14650455、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8058Hexane溶媒

実験手順

[2-(1-cyclohexenyl)-4-oxo-4H-[1]-benzopyran-8-yl]acetic acid (100 mg) and triethylamine (53 mg) were added to dichloromethane (2ml). After addition of diphenylphosphoryl azide (145 mg) with stirring under ice cooling, the mixture was stirred at room temperature for 1 hour. Conc. aqueous ammonia (5 ml) was added to the reaction mixture and stirring was further continued for 1 hour. Hexane (5 ml) was added and crystals deposited were filtered off. The crystals were recrystallized from dichloromethane and methanol to obtain the title compound as needles, m.p. 244°-245° C., yield 64 mg (64.6%).

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hour
  2. stirringstirring
  3. filtrationcrystals deposited were filtered off
  4. customThe crystals were recrystallized from dichloromethane and methanol

出典と根拠

ORDレコード
ord-5173607d421f47efa01fc73c817cc319
出典データセット
uspto-grants-1990_02
特許番号
US04904690

反応ノート

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