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Triethylamine → Methyl 4-{{4-[2-(1-ethyl-6,11-dihydro-5-methyl-6-oxo-5h-dipyrido[3,2-b:2',3'-e][1,4]diazepin-8-yl)ethoxy]-3-methylbenzoyl}amino}benzoate

HRID 393294
ノート
印刷プレビュー

反応式

HRID 393294 の反応式
C([N:3]1[C:9]2[N:10]=[CH:11][C:12]([CH2:14][CH2:15][O:16][C:17]3[CH:25]=[CH:24][C:20]([C:21](Cl)=[O:22])=[CH:19][C:18]=3[CH3:26])=[CH:13][C:8]=2[C:7](=[O:27])[N:6]([CH3:28])[C:5]2[CH:29]=[CH:30][CH:31]=[N:32][C:4]1=2)C.[NH2:33][C:34]1[CH:43]=[CH:42][C:37]([C:38]([O:40][CH3:41])=[O:39])=[CH:36][CH:35]=1.[CH3:44][CH2:45]N(CC)CC>C(Cl)Cl.CCOC(C)=O>[CH2:44]([N:32]1[C:4]2[NH:3][C:9]3[N:10]=[CH:11][C:12]([CH2:14][CH2:15][O:16][C:17]4[CH:25]=[CH:24][C:20]([C:21]([NH:33][C:34]5[CH:35]=[CH:36][C:37]([C:38]([O:40][CH3:41])=[O:39])=[CH:42][CH:43]=5)=[O:22])=[CH:19][C:18]=4[CH3:26])=[CH:13][C:8]=3[C:7](=[O:27])[N:6]([CH3:28])[C:5]=2[CH:29]=[CH:30][CH2:31]1)[CH3:45]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 12082Methyl 4-aminobenzoateHCID 226488664-[2-(11-Ethyl-6,11-dihydro-5-methyl-6-oxo-5h-dipyrido[3,2-b:2',3'-e][1,4]diazepin-8-yl)ethoxy]-3-methyl benzoyl chloride

生成物 1

HCID 22648879Methyl 4-{{4-[2-(1-ethyl-6,11-dihydro-5-methyl-6-oxo-5h-dipyrido[3,2-b:2',3'-e][1,4]diazepin-8-yl)ethoxy]-3-methylbenzoyl}amino}benzoate収率 76%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-[2-(11-ethyl-6,11-dihydro-5-methyl-6-oxo-5H-dipyrido[3,2-b:2′,3′-e][1,4]diazepin-8-yl)ethoxy]-3-methylbenzoyl chloride (47.0 mg, 0.11 mmol), methyl 4-aminobenzoate (15.8 mg, 0.11 mmol) and Et3N (15.3 μL, 0.11 mmol) in CH2Cl2 (4 mL) was stirred at 25° C. for 5 h. The reaction mixture was diluted with EtOAc and the resulting solution was successively washed with aqueous saturated NaHCO3 solution and brine, dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (Hexane:EtOAc, 1:1) to give the title compound (45 mg, 76% yield) as a white solid.

後処理

  1. washthe resulting solution was successively washed with aqueous saturated NaHCO3 solution and brine
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by flash chromatography (Hexane:EtOAc, 1:1)

出典と根拠

ORDレコード
ord-ba01f49ec2594debaa1a45705993fdce
出典データセット
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06806265B2

反応ノート

読み込み中…

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