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Potassium Iodide → HCID 21412235, 화합물

HRID 259527
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HRID 259527 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:17]=[CH:16][C:15]2[C:18]3[C:8]=1[CH2:9][CH2:10][C:11]=3[CH:12]=[CH:13][C:14]=2[C:19](=[O:24])[CH2:20][CH2:21][CH2:22]Cl)=[O:6].[I-].[K+].[CH2:27]([NH:29][CH2:30][CH3:31])[CH3:28]>O1CCCC1>[ClH:1].[ClH:1].[CH2:27]([N:29]([CH2:30][CH3:31])[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:17]=[CH:16][C:15]2[C:18]3[C:8]=1[CH2:9][CH2:10][C:11]=3[CH:12]=[CH:13][C:14]=2[C:19](=[O:24])[CH2:20][CH2:21][CH2:22][N:29]([CH2:30][CH3:31])[CH2:27][CH3:28])=[O:6])[CH3:28]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 8021DiethylamineHCID 214122473,6-Bis(4-chlorobutyryl)acenaphthene

생성물 1

HCID 21412235HCID 21412235, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
120 °C

실험 절차

A mixture of 36.1 g (0.10 mole) of 3,6-bis(4-chlorobutyryl)acenaphthene, 2 g of potassium iodide, 100 ml of diethylamine and 100 ml of tetrahydrofuran is placed in a bomb and heated for 24 hours at 120° C. Upon cooling, the mixture is filtered and the filtrate evaporated to dryness. The cooled residue is dissolved in 300 ml of 10% hydrochloric acid, filtered and the acid filtrate made alkaline with a 20% sodium hydroxide solution. The resulting 3,6-bis[4-(diethylamino)butyryl]acenaphthene so obtained is filtered and subsequently recrystallized from a methanol-ethyl acetate solution.

후처리

  1. temperatureUpon cooling
  2. filtrationthe mixture is filtered
  3. customthe filtrate evaporated to dryness
  4. dissolutionThe cooled residue is dissolved in 300 ml of 10% hydrochloric acid
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-e3c5fc95c46749f6ada6a31958eea1a5
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04038400

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