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Sodium Iodide → (3-carbamoyl)-5-(octadecyloxy)phenyl-N-[2-(phenylmethoxy)-2-oxoethyl]glycine phenylmethyl ester

HRID 1110264
ノート
印刷プレビュー

反応式

HRID 1110264 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH:10]=1)[C:5]([NH2:7])=[O:6].Br[CH2:31][C:32]([O:34][CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:33].CN(C)[C:44]1[C:53]2[C:48](=[CH:49][CH:50]=[CH:51][C:52]=2N(C)C)C=CC=1.[I-].[Na+]>C(#N)C.CN(C=O)C>[C:36]1([CH2:35][O:34][C:32](=[O:33])[CH2:31][N:1]([C:2]2[CH:10]=[C:9]([O:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])[CH:8]=[C:4]([C:5](=[O:6])[NH2:7])[CH:3]=2)[CH2:31][C:32](=[O:33])[O:34][CH2:44][C:53]2[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=2)[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 62576Benzyl bromoacetateHCID 88675Proton spongeHCID 19389096HCID 19389096、化合物

生成物 1

HCID 19388969(3-carbamoyl)-5-(octadecyloxy)phenyl-N-[2-(phenylmethoxy)-2-oxoethyl]glycine phenylmethyl ester収率 43.2%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6342Acetonitrile溶媒

実験手順

A mixture of 3.0 g (7.4 mmol) of 3-amino-5-(octadecyloxy)benzamide, 3.6 ml (22 mmol) of benzyl bromoacetate, 4.0 g (18.5 mmol) of 1,8-bis(dimethylamino)naphthalene and 0.3 g (2.1 mmol) of sodium iodide in 60 ml of acetonitrile and 20 ml of DMF was stirred and heated at reflux under argon for 48 hours. The solvents were removed at reduced pressure and the residue was dissolved in ethyl acetate. The extract was washed with 0.05N HCl, with NaHCO3 solution, dried and concentrated at reduced pressure to a solid. Purification by HPLC using 20% ethyl acetate-toluene gave 2.24 g (43% yield, mp 112°-114°) of N-[(3-carbamoyl)-5-(octadecyloxy)phenyl]-N-[2-oxo-2-(phenylmethoxy)ethyl]glycine phenylmethyl ester.

後処理

  1. temperatureheated
  2. temperatureat reflux under argon for 48 hours
  3. customThe solvents were removed at reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washThe extract was washed with 0.05N HCl, with NaHCO3 solution
  6. customdried
  7. concentrationconcentrated at reduced pressure to a solid
  8. customPurification by HPLC

出典と根拠

ORDレコード
ord-91b975c58ddb481e85edc92fee6c78f2
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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