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Pyridine → HCID 178445143, 화합물

HRID 2198547
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HRID 2198547 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH:9][C:10]([N:12]([CH3:25])[C:13]2[CH:21]=[CH:20][CH:19]=[C:18]3[C:14]=2[C:15](=[O:24])[N:16]([CH3:23])[C:17]3=[O:22])=[O:11])=[CH:4][CH:3]=1.N1C=CC=CC=1.[C:32](Cl)(=[O:38])[CH2:33][CH2:34][CH2:35][CH2:36][CH3:37]>C(#N)C>[C:32]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH:9][C:10]([N:12]([CH3:25])[C:13]2[CH:21]=[CH:20][CH:19]=[C:18]3[C:14]=2[C:15](=[O:24])[N:16]([CH3:23])[C:17]3=[O:22])=[O:11])=[CH:4][CH:3]=1)(=[O:38])[CH2:33][CH2:34][CH2:35][CH2:36][CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 67340Hexanoyl chlorideHCID 178481327HCID 178481327, 화합물

생성물 1

HCID 178445143HCID 178445143, 화합물수율 30.5%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

1-p-Aminophenyl-4-methyl-4-(2-methyl-1,3-dioxoisoindolin-4-yl)semicarbazide (1.5 g, 4.5 mmole) and pyridine (1 ml) were dissolved in 30 ml of acetonitrile under nitrogen and cooled to +5° C. in an ice bath. Hexanoyl chloride (0.6 g, 4.5 mmole) in 5 ml of acetonitrile was added dropwise. The mixture was stirred 11/2 hours at ice-bath temperature. The resulting solid was filtered to give 0.6 g of product, m.p. 115°-118° C. Recrystallization from acetonitrile and ethyl acetate gave 0.32 g (16% yield) of product, m.p. 147°-149° C.

후처리

  1. temperaturecooled to +5° C. in an ice bath
  2. filtrationThe resulting solid was filtered

출처 및 근거

ORD 기록
ord-8fae3885a0de4347ade7d9a777d647ed
출처 데이터셋
uspto-grants-1982_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04358525

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