4-Methylmorpholine → Boc-MePhe-Leu-OMe

HRID 1390156

反応式

HRID 1390156 の反応式
[C:1]([N:8]([CH3:20])[C@H:9]([C:17]([OH:19])=O)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].CN1CCOCC1.C(OC(Cl)=O)C(C)C.[NH:36](Cl)[C@H:37]([C:42]([O:44][CH3:45])=[O:43])[CH2:38][CH:39]([CH3:41])[CH3:40]>C1COCC1.CN(C=O)C.C(OC(=O)C)C>[C:1]([N:8]([CH3:20])[C@H:9]([C:17]([NH:36][C@H:37]([C:42]([O:44][CH3:45])=[O:43])[CH2:38][CH:39]([CH3:41])[CH3:40])=[O:19])[CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]

参加物

8

反応物 4

HCID 79724-Methylmorpholine2 回HCID 62365Isobutyl chloroformateHCID 7010602Boc-N-Me-Phe-OHHCID 88276507HCl-LeuOMe

生成物 1

HCID 13918317Boc-MePhe-Leu-OMe

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 28 g of Boc-MePhe-OH and 11.2 ml of N-methylmorpholine in 400 ml of THF are added 13.2 ml of chloroformic acid isobutyl ester at -25°. After 5 minutes, at -25°, 18 g of HCl-Leu-OMe and 11.2 ml of N-methylmorpholine in 200 ml of DMF are added to the solution. After 2 hours, at -15°, the mixture is diluted with ethylacetate, washed with dilute aqueous KHCO3 solution, hydrochloric acid, water, dried and the solvent removed under vacuum to yield the title compound as a viscous oil.

後処理

  1. waitAfter 2 hours
  2. washwashed with dilute aqueous KHCO3 solution, hydrochloric acid, water
  3. customdried
  4. customthe solvent removed under vacuum

出典と根拠

ORDレコード
ord-eb8cf7f9edb54ce4a6914eb9f723860a
出典データセット
uspto-grants-1981_01
特許番号
US04247543

関連ノート

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