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Proton sponge → HCID 18408893、化合物

HRID 993043
ノート
印刷プレビュー

反応式

HRID 993043 の反応式
Cl.Cl.[O:3]=[C:4]1[CH2:9][N:8]([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH2:7][CH2:6][N:5]1[CH2:16][C:17]([C:19]1[CH:31]=[CH:30][C:22]([O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:21][CH:20]=1)=[O:18].CN(C1C2C(N(C)C)=CC=CC=2C=CC=1)C.Cl[C:49]([O:51][CH:52]([Cl:56])[CH:53](C)C)=[O:50]>C(Cl)Cl.C(OCC)(=O)C.O>[Cl:56][CH:52]([O:51][C:49]([N:13]1[CH2:12][CH2:11][CH:10]([N:8]2[CH2:7][CH2:6][N:5]([CH2:16][C:17]([C:19]3[CH:31]=[CH:30][C:22]([O:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])=[CH:21][CH:20]=3)=[O:18])[C:4](=[O:3])[CH2:9]2)[CH2:15][CH2:14]1)=[O:50])[CH3:53]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 88675Proton spongeHCID 27333261-Chloro-2-Methylpropyl ChloroformateHCID 18408903HCID 18408903、化合物

生成物 1

HCID 18408893HCID 18408893、化合物収率 77.7%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒
2 回
HCID 8857Ethyl Acetate溶媒

反応条件

温度
-40 °C

実験手順

To a solution of 0.75 g of ethyl 4-[[2-oxo-4-(piperidin-4-yl)-piperazin-1-yl]acetyl]phenoxyacetate dihydrochloride synthesized according to the method described in WO962503 in 16 ml of methylene chloride was added 1.11 g of proton sponge under ice-cooling. After stirring for 5 minutes, the mixture was cooled to −40° C., and a solution of 0.322 g of 1-chloro-2-methylpropyl chloroformate in 2 ml of methylene chloride. After stirring for 45 minutes, the reaction mixture was diluted with ethyl acetate and water, and the organic layer was separated. The aqueous layer was extracted with ethyl acetate. The organic layer collected was washed with saturated aqueous saline, dried over sodium sulfate, and the solvent was removed by distillation. The residue was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1-40:1) to give 0.624 g (74%) of ethyl 4-[[4-[1-(1-chloroethoxycarbonyl)piperidin-4-yl]-2-oxopiperazin-1-yl]acetyl]phenoxyacetate.

後処理

  1. temperaturecooling
  2. stirringAfter stirring for 45 minutes
  3. customthe organic layer was separated
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. customThe organic layer collected
  6. washwas washed with saturated aqueous saline
  7. dry with materialdried over sodium sulfate
  8. customthe solvent was removed by distillation
  9. customThe residue was purified by chromatography on a silica gel column (methylene chloride:methanol=50:1-40:1)

出典と根拠

ORDレコード
ord-a467cc34290f4d8f90f9cc90b731fc2c
出典データセット
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06472397B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート