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Hexane → HCID 15917440, 화합물

HRID 648096
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HRID 648096 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[CH2:6][C:7]3([O:18][C:4]=2[CH:3]=1)[C:16]1[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH2:10][N:9](C)[CH2:8]3.Cl[C:22]([O:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:23].CCCCCC>ClCCl>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[CH2:6][C:7]3([O:18][C:4]=2[CH:3]=1)[C:16]1[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=1)[CH2:10][N:9]([C:22]([O:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:23])[CH2:8]3
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8058HexaneHCID 15891Phenyl chloroformateHCID 15917438HCID 15917438, 화합물

생성물 1

HCID 15917440HCID 15917440, 화합물수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To an ice cold solution of 6-chloro-2'-methylspiro[benzofuran-2(3H),4'(2'H)-isoquinoline] (5.0 g) in dichloromethane (150 ml) is slowly added dropwise phenyl chloroformate (3.7 g) in dichloromethane (20 ml). The mixture is stirred at ambient temperature overnight. Removal of the solvent in vacuo yields an orange oil which solidifies upon trituration with hexane. An analytical sample is twice recrystallized from hexane to yield product as a solid (6.6 g, 99%), mp 138°-140°.

후처리

  1. customRemoval of the solvent in vacuo
  2. customyields an orange oil which
  3. customAn analytical sample is twice recrystallized from hexane

출처 및 근거

ORD 기록
ord-076e426143af4439a000c173bacff03b
출처 데이터셋
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04410699

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