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1,2-Dichloroethane → HCID 53834349、化合物

HRID 1858574
ノート
印刷プレビュー

反応式

HRID 1858574 の反応式
[NH2:1][CH2:2][C:3]1[CH:29]=[CH:28][CH:27]=[CH:26][C:4]=1[CH2:5][O:6][CH:7]1[CH:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:11][CH2:10][N:9]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:8]1.C(N(CC)CC)C.[C:37](O)(=[O:44])[C:38]1[CH:43]=[CH:42][CH:41]=[N:40][CH:39]=1.C(Cl)CCl>C(Cl)Cl.CN(C)C1C=CN=CC=1>[C:13]1([CH:12]2[CH2:11][CH2:10][N:9]([C:19]([O:21][C:22]([CH3:24])([CH3:25])[CH3:23])=[O:20])[CH2:8][CH:7]2[O:6][CH2:5][C:4]2[CH:26]=[CH:27][CH:28]=[CH:29][C:3]=2[CH2:2][NH:1][C:37]([C:38]2[CH:39]=[N:40][CH:41]=[CH:42][CH:43]=2)=[O:44])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=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 111,2-DichloroethaneHCID 938Nicotinic AcidHCID 8471TriethylamineHCID 54186768HCID 54186768、化合物

生成物 1

HCID 53834349HCID 53834349、化合物収率 53%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒
2 回

実験手順

A solution of 150 mg (0.38 mmol) of tert-butyl (3RS,4RS)-3-(2-aminomethyl-benzyloxy)-4-phenyl-piperidine-1-carboxylate in 2 ml of methylene chloride was treated with 229 mg (2.26 mmol) of triethylamine, 139 mg (1.05 mmol) of nicotinic acid, 216 mg (1.13 mmol) of EDC and 10 mg (0.08 mmol) of 4-dimethylaminopyridine and the mixture was stirred at room temperature for 24 hours. Thereafter, the reaction solution was diluted with methylene chloride and washed with a saturated sodium hydrogen carbonate solution. The organic phase was separated, dried over sodium sulphate and evaporated under reduced pressure. The residue was chromatographed on silica gel using ethyl acetate as the eluent. There were obtained 100 mg (53% of theory) of tert-butyl (3RS,4RS)-4-phenyl-3-(2-{[(pyridine-3-carbonyl)-amino]-methyl}-benzyloxy)-piperidine-1-carboxylate as a colourless solid; MS: 502 (M+H)+.

後処理

  1. washwashed with a saturated sodium hydrogen carbonate solution
  2. customThe organic phase was separated
  3. dry with materialdried over sodium sulphate
  4. customevaporated under reduced pressure
  5. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-c781f49af91b4351aaf48736124e7c00
出典データセット
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06150526

反応ノート

読み込み中…

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