Ethylmorpholine → HCID 67806908、化合物

HRID 467133ノート

反応式

HRID 467133 の反応式
[NH:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[C@H:2]([C:4]([OH:6])=O)[CH3:3].C(N1CCOCC1)C.C1C=CC2N(O)N=NC=2C=1.Cl.[CH2:33]([O:40][C:41]([CH:43]1[CH2:51][CH:50]2[CH:45]([CH2:46][CH2:47][CH2:48][CH2:49]2)[NH:44]1)=[O:42])[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C=O>[CH2:33]([O:40][C:41]([CH:43]1[CH2:51][CH:50]2[CH:45]([CH2:46][CH2:47][CH2:48][CH2:49]2)[N:44]1[C:4](=[O:6])[C@H:2]([CH3:3])[NH:1][C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])=[O:42])[C:34]1[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=1

参加物

7

反応物 5

HCID 7525EthylmorpholineHCID 10868DicyclohexylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 85082Tert-butoxycarbonylalanineHCID 19902522Benzyl octahydro-1H-indole-2-carboxylate hydrochloride

生成物 1

HCID 67806908HCID 67806908、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

19 g of Boc-Ala-OH are dissolved in 100 ml of dimethylformamide, and 13 ml of N-ethylmorpholine, 13.5 g of HOBt and 29.6 g of octahydroindole-2-carboxylic acid benzyl ester hydrochloride are added to the solution. The mixture is cooled in an ice bath, 21 g of dicyclohexylcarbodiimide are added to it, and it is stirred for 15 hours at room temperature. The precipitated urea is filtered off under suction, and the filtrate is concentrated in vacuo and taken up in ethyl acetate. The solution is extracted 3 times in each case with aqueous KHSO4 solution, KHCO3 solution and saturated NaCl solution and the organic phase is concentrated in vacuo.

後処理

  1. temperatureThe mixture is cooled in an ice bath
  2. filtrationThe precipitated urea is filtered off under suction
  3. concentrationthe filtrate is concentrated in vacuo
  4. extractionThe solution is extracted 3 times in each case with aqueous KHSO4 solution, KHCO3 solution and saturated NaCl solution
  5. concentrationthe organic phase is concentrated in vacuo

出典と根拠

ORDレコード
ord-0b640097c12049afbc5490456d26cedd
出典データセット
uspto-grants-1992_10
特許番号
US05158959

反応ノート

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