Hydrochloric Acid → 1-(7,8-Dimethoxy2,3-dihydro-1-benzoxepin-4-ylcarbonyl)-2-methoxymethyl4-(3,4,5-trimethoxybenzoyl)piperazine

HRID 358777노트

반응식

HRID 358777 반응식
[CH3:1][O:2][C:3]1[C:4]([O:17][CH3:18])=[CH:5][C:6]2[O:12][CH2:11][CH2:10][C:9]([C:13](Cl)=[O:14])=[CH:8][C:7]=2[CH:16]=1.[CH3:19][O:20][CH2:21][CH:22]1[NH:27][CH2:26][CH2:25][N:24]([C:28](=[O:41])[C:29]2[CH:34]=[C:33]([O:35][CH3:36])[C:32]([O:37][CH3:38])=[C:31]([O:39][CH3:40])[CH:30]=2)[CH2:23]1.Cl.C(N(CC)CC)C>ClCCl>[CH3:1][O:2][C:3]1[C:4]([O:17][CH3:18])=[CH:5][C:6]2[O:12][CH2:11][CH2:10][C:9]([C:13]([N:27]3[CH2:26][CH2:25][N:24]([C:28](=[O:41])[C:29]4[CH:34]=[C:33]([O:35][CH3:36])[C:32]([O:37][CH3:38])=[C:31]([O:39][CH3:40])[CH:30]=4)[CH2:23][CH:22]3[CH2:21][O:20][CH3:19])=[O:14])=[CH:8][C:7]=2[CH:16]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 104682747,8-Dimethoxy-2,3-dihydro-1-benzoxepine-4-carbonyl chlorideHCID 200665933-Methoxymethyl-1-(3,4,5-trimethoxybenzoyl)piperazine

생성물 1

HCID 216252111-(7,8-Dimethoxy2,3-dihydro-1-benzoxepin-4-ylcarbonyl)-2-methoxymethyl4-(3,4,5-trimethoxybenzoyl)piperazine

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 7,8-dimethoxy-2,3-dihydro-1-benzoxepine-4-carbonyl chloride (300 mg) in dichloromethane (10 ml) is added dropwise, taking 30 minutes under ice-cooling while stirring, to a mixture of 3-methoxymethyl-1-(3,4,5-trimethoxybenzoyl)piperazine×hydrochloride (400 mg) obtained in Reference Example 6, triethylamine (1 ml) and dichloromethane (30 ml). The reaction mixture is washed with an aqueous solution of citric acid and an aqueous solution of sodium hydrogencarbonate, then dried over magnesium sulfate, followed by concentration. The concentrate is subjected to a silica gel column chromatography (eluent: ethyl acetate-methanol =95:5) to afford 1-(7,8-dimethoxy2,3-dihydro-1-benzoxepin-4-ylcarbonyl) -2-methoxymethyl4-(3,4,5-trimethoxybenzoyl)piperazine (520 mg) as colorless crystals, m.p. 142° C.

후처리

  1. temperaturecooling
  2. washThe reaction mixture is washed with an aqueous solution of citric acid
  3. dry with materialan aqueous solution of sodium hydrogencarbonate, then dried over magnesium sulfate
  4. concentrationfollowed by concentration

출처 및 근거

ORD 기록
ord-d1776094d76841359daecf25d73335d5
출처 데이터셋
uspto-grants-1991_03
특허 번호
US04997836

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