4-Methylmorpholine → Alanine--lysine (1/1)

HRID 1291973

反応式

HRID 1291973 の反応式
CN1CCOCC1.C([N:25](C(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O)[C@H:26]([C:32]([OH:34])=[O:33])[CH2:27][CH2:28][CH2:29][CH2:30][NH2:31])(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O.F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1.ON1C2C=CC=CC=2N=N1.N[C@H](C([NH:104][C@H:105]([C:107]([OH:109])=[O:108])[CH3:106])=O)CCCCN>CN(C=O)C>[NH2:25][C@H:26]([C:32]([OH:34])=[O:33])[CH2:27][CH2:28][CH2:29][CH2:30][NH2:31].[NH2:104][C@H:105]([C:107]([OH:109])=[O:108])[CH3:106]

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 2724699PyBOPHCID 7010504Lys-AlaHCID 23385649Bis-fmoc-lysine

生成物 1

HCID 168589Alanine--lysine (1/1)

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The resin is suspended in 70 ml of activator solution (5% N-methyl-morpholine in DMF). Thereafter, added to the suspension are 8.2 g (14 mmoles) of bis-Fmoc-lysine, 7.28 g of coupling agent, benzotriazol-1-yl-oxy-tris-pyrro-lidinophosphonium hexafluorophosphate (PyBOP), and 2.14 g of catalyst, 1-hydroxybenzotriazole (HOBT). The reaction medium is mixed for 90 minutes and the resultant product is (Fmoc)2 -Lys-Ala-resin, i.e., (Fmoc)2 -K-A-resin. The product of the coupling reaction is washed 3 times with DCM, 1 time with methanol and 5 times with DMF and then subjected to deprotection using a mixture of 30% piperidine, 35% toluene and 35% DMF. The product obtained from the deprotection is Lys-Ala-resin (K-A-resin). This product is washed 5 times with DMF, 1 time with methanol and 3 times with DCM.

後処理

  1. additionThereafter, added to the suspension
  2. additionThe reaction medium is mixed for 90 minutes
  3. customThe product of the coupling reaction
  4. washis washed 3 times with DCM, 1 time with methanol and 5 times with DMF
  5. additiona mixture of 30% piperidine, 35% toluene and 35% DMF
  6. customThe product obtained from the deprotection
  7. washThis product is washed 5 times with DMF, 1 time with methanol and 3 times with DCM

出典と根拠

ORDレコード
ord-b22208ff4b23440f87a75998bbb9e3d7
出典データセット
uspto-grants-1998_05
特許番号
US05756066

関連ノート

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