Cyclohexyl isocyanate → HCID 178418526, 화합물

HRID 3796

반응식

HRID 3796 반응식
[CH:1]1([N:7]=[C:8]=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:10][C:11]1[CH:27]=[CH:26][C:14]([CH2:15][N:16]2[CH2:21][CH2:20][N:19]([CH2:22][CH2:23][CH2:24][SH:25])[CH2:18][CH2:17]2)=[CH:13][CH:12]=1>C(Cl)Cl>[ClH:10].[ClH:10].[CH:1]1([NH:7][C:8](=[SH:25][CH2:24][CH2:23][CH2:22][N:19]2[CH2:20][CH2:21][N:16]([CH2:15][C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:27][CH:26]=3)[CH2:17][CH2:18]2)[OH:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 18502Cyclohexyl isocyanateHCID 137311173-[4-(4-Chlorobenzyl)piperazin-1-yl]propanethiol

생성물 1

HCID 178418526HCID 178418526, 화합물수율 100.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1.0 g of cyclohexyl isocyanate, 2.1 g of 3-[4-(4-chlorobenzyl)piperazin-1-yl]propanethiol and 10 ml of methylene chloride was stirred at room temperature overnight and then concentrated in vacuo. The residue crystallized upon standing. The product was recrystallized from aqueous ethanol, dissolved in ether, and the ethanol solution was dried (magnesium sulfate). The salt was then precipitated with ethereal hydrochloric acid and recrystallized twice from aqueous ethanol to give 1.2 g (30% of theory) of N-cyclohexyl-S-{3-[4-(4-chlorobenzyl)piperazin-1-yl]propyl}thiocarbamate dihydrochloride as a white crystalline solid, M.p. >165° C. (dec.).

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue crystallized
  3. customThe product was recrystallized from aqueous ethanol
  4. dissolutiondissolved in ether
  5. dry with materialthe ethanol solution was dried (magnesium sulfate)
  6. customThe salt was then precipitated with ethereal hydrochloric acid
  7. customrecrystallized twice from aqueous ethanol

출처 및 근거

ORD 기록
ord-9d1937c896e54cb4b8977e4368ead391
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

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