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Dichloromethane → N-(2-diethylaminoethoxy-2-oxoethyl)-N-[3,5-bis(decyloxy)phenyl]glycine monohydrochloride salt

HRID 1110234
ノート
印刷プレビュー

反応式

HRID 1110234 の反応式
[CH2:1]([O:11][C:12]1[CH:13]=[C:14]([N:29]2[CH2:34][C:33](=[O:35])[O:32][C:31](=[O:36])[CH2:30]2)[CH:15]=[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:37]([N:39]([CH2:43][CH3:44])[CH2:40][CH2:41][OH:42])[CH3:38].C(Cl)[Cl:46]>>[ClH:46].[CH2:37]([N:39]([CH2:43][CH3:44])[CH2:40][CH2:41][O:42][C:33](=[O:35])[CH2:34][N:29]([C:14]1[CH:15]=[C:16]([O:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[CH:17]=[C:12]([O:11][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH:13]=1)[CH2:30][C:31]([OH:36])=[O:32])[CH3:38]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 7497DiethylethanolamineHCID 193890794-[3,5-Bis(decyloxy)phenyl]2,6-morpholinedione

生成物 1

HCID 21808303N-(2-diethylaminoethoxy-2-oxoethyl)-N-[3,5-bis(decyloxy)phenyl]glycine monohydrochloride salt収率 82%

実験手順

A solution of 0.43 g (0.85 mmol) of 4-[3,5-bis(decyloxy)phenyl]2,6-morpholinedione and 0.23 ml (1.71 mmol) of N,N-diethylethanolamine in 40 ml of methylene chloride was kept at room temperature for 3.5 days. The solvent was removed at reduced pressure and the residue was dissolved in ethyl acetate. The extract was washed with water and then with 0.5N HCl, dried and concentrated at reduced pressure to a yellow foam which was dissolved in ether and cooled. Filtration gave 0.46 g (82% yield, mp 89°-91°) of N-(2-diethylaminoethoxy-2-oxoethyl)-N-[3,5-bis(decyloxy)phenyl]glycine monohydrochloride salt.

後処理

  1. customThe solvent was removed at reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialwith 0.5N HCl, dried
  5. concentrationconcentrated at reduced pressure to a yellow foam which
  6. dissolutionwas dissolved in ether
  7. temperaturecooled
  8. filtrationFiltration

出典と根拠

ORDレコード
ord-783fcb93613a4787b0ddd33cfa3e5717
出典データセット
uspto-grants-1994_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05324747

反応ノート

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