Ammonia → HCID 14650455, 화합물

HRID 1200187노트

반응식

HRID 1200187 반응식
[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

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 14650449HCID 14650449, 화합물

생성물 1

HCID 14650455HCID 14650455, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8058Hexane용매

실험 절차

[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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5173607d421f47efa01fc73c817cc319
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904690

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