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Sodium Bicarbonate → 2-{4-[4-(4-Hydroxyphenyl)-1-piperazinyl]butyl}naphtho[1,8-cd]isothiazole 1,1-dioxide

HRID 1087514
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반응식

HRID 1087514 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][N:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[C:14]3[CH:15]=[CH:16][CH:17]=[C:8]([C:9]=23)[S:7]1(=[O:19])=[O:18].Br.Br.[OH:22][C:23]1[CH:28]=[CH:27][C:26]([N:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[CH:25][CH:24]=1.C(=O)(O)[O-].[Na+]>CN(C)C=O.O1CCCC1>[OH:22][C:23]1[CH:24]=[CH:25][C:26]([N:29]2[CH2:34][CH2:33][N:32]([CH2:2][CH2:3][CH2:4][CH2:5][N:6]3[C:10]4[CH:11]=[CH:12][CH:13]=[C:14]5[CH:15]=[CH:16][CH:17]=[C:8]([C:9]=45)[S:7]3(=[O:19])=[O:18])[CH2:31][CH2:30]2)=[CH:27][CH:28]=1
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참가 물질

6

반응물 3

HCID 516892Sodium BicarbonateHCID 2723591p-(1-Piperazinyl)phenol dihydrobromideHCID 28004062-(4-Chlorobutyl)-1lambda6-naphtho[1,8-CD]isothiazole-1,1(2H)-dione

생성물 1

HCID 198170802-{4-[4-(4-Hydroxyphenyl)-1-piperazinyl]butyl}naphtho[1,8-cd]isothiazole 1,1-dioxide수율 69.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide
용매
HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

The experiment is carried out as in Example 1, starting with 2-(4-chlorobutyl)naphtho[1,8-cd]isothiazole 1,1-dioxide (3 g), 4-(4-hydroxyphenyl)piperazine dihydrobromide (3.8 g) and sodium bicarbonate (2.8 g) in a mixture of dimethylformamide (30 cc) and tetrahydrofuran (20 cc). The mixture is heated for 5 hours at boiling point, then cooled to a temperature of about 20° C. After purification by recrystallization from boiling acetone (215 cc), 2-{4-[4-(4-hydroxyphenyl)-1-piperazinyl]butyl}naphtho[1,8-cd]isothiazole 1,1-dioxide (3.1 g) is obtained, m.p. 195° C.

후처리

  1. temperatureThe mixture is heated for 5 hours
  2. customAfter purification
  3. customby recrystallization

출처 및 근거

ORD 기록
ord-178bad3f90ec4c2abe8a09e06816e2c4
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05036075

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