3-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol → HCID 131715247, 화합물

HRID 2309028

반응식

HRID 2309028 반응식
[Cl:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][N:7]2[CH2:13][CH2:12][CH2:11][N:10]([CH2:14][CH2:15][CH2:16][SH:17])[CH2:9][CH2:8]2)=[CH:4][CH:3]=1>[OH-].[Na+]>[ClH:1].[ClH:1].[ClH:1].[ClH:1].[CH2:14]([N:10]1[CH2:11][CH2:12][CH2:13][N:7]([CH2:6][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:19][CH:18]=2)[CH2:8][CH2:9]1)[CH2:15][CH2:16][S:17][S:17][CH2:16][CH2:15][CH2:14][N:10]1[CH2:11][CH2:12][CH2:13][N:7]([CH2:6][C:5]2[CH:18]=[CH:19][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:8][CH2:9]1

참가 물질

3

반응물 1

HCID 201531743-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol

생성물 1

HCID 131715247HCID 131715247, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 3-[4-(4-chlorobenzyl)homopiperazin-1-yl]-propanethiol (4.0 g) and 2N sodium hydroxide (50 ml) is stirred at room temperature for 8 days. The product is extracted with ether, dried, and concentrated to give a yellow oil, which is purified on a silica gel column (methylene chloride:methanol, 95:5). The resulting yellow oil (1.5 g) is dissolved in ether and the salt precipitated with ethereal hydrochloric acid. Recrystallization from ethanol provided 1,1'-(dithiodi-3,1-propanediyl)bis[4-(4-chlorobenzyl) homopiperizine] tetrahydrochloride as a white crystalline solid, m.p. >170° (dec.).

후처리

  1. extractionThe product is extracted with ether
  2. customdried
  3. concentrationconcentrated
  4. customto give a yellow oil, which
  5. customis purified on a silica gel column (methylene chloride:methanol, 95:5)
  6. dissolutionThe resulting yellow oil (1.5 g) is dissolved in ether
  7. customthe salt precipitated with ethereal hydrochloric acid
  8. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-be17ec7fba0a48c082c630510fedb7ca
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692448

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