Hydrochloric Acid → HCID 20287077, 화합물

HRID 127473

반응식

HRID 127473 반응식
Br[CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]([OH:15])=[C:9]([CH:14]=1)[C:10]([O:12][CH3:13])=[O:11])=[O:4].[CH3:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.C(N(CC)CC)C.Br.C(N(CC)CC)C.[ClH:44]>O1CCCC1.C(OCC)C>[ClH:44].[ClH:44].[OH:15][C:8]1[CH:7]=[CH:6][C:5]([C:3](=[O:4])[CH2:2][N:26]2[CH2:27][CH2:28][N:23]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[CH3:16])[CH2:24][CH2:25]2)=[CH:14][C:9]=1[C:10]([O:12][CH3:13])=[O:11]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 919652-MeppHCID 2734074Triethylammonium bromideHCID 11601501Methyl 5-(2-bromoacetyl)-2-hydroxybenzoate

생성물 1

HCID 20287077HCID 20287077, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 10.9 g (0.04 mol) of methyl 5-(2-bromoacetyl)-2-hydroxybenzoate in 100 ml of dry tetrahydrofuran is added dropwise over 4 hours to a stirred solution of 7.1 g (0.04 mol) of 1-(2-methylphenyl)piperazine and 4.0 g (0.04 mol) of triethylamine in 75 ml of tetrahydrofuran at room temperature. Stirring is continued for 2-12 hours or until the theoretical amount (7.3 g) of triethylamine hydrobromide precipitates. The precipitates is removed by filtration and the filtrate is evaporated to dryness. Addition of 2 equivalents of methanolic HCl and precipitation by addition of ethyl ether at room temperature affords the crude methyl 2-hydroxy-5-[2-[4-(2-methylphenyl)-1-piperazinyl]acetyl]benzoate dihydrochloride (9.4 g). Attempts to purify this product by recrystallization frequently led to decomposition and were subsequently avoided.

후처리

  1. customprecipitates
  2. customThe precipitates is removed by filtration
  3. customthe filtrate is evaporated to dryness

출처 및 근거

ORD 기록
ord-35f46730076441c895e1fb9d05cddd04
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04255575

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