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Trifluoroacetic acid → HCID 23002643、化合物

HRID 1371536
ノート
印刷プレビュー

反応式

HRID 1371536 の反応式
F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=N1.C(OC([NH:35][CH:36]([CH2:40][C:41]1[CH:46]=[CH:45][C:44]([C:47]#[N:48])=[CH:43][CH:42]=1)[C:37]([OH:39])=O)=O)(C)(C)C.N1CCCC1.C(N1CCOCC1)C.[C:62]([OH:68])([C:64]([F:67])([F:66])[F:65])=[O:63]>CN(C=O)C.C(Cl)Cl>[F:65][C:64]([F:67])([F:66])[C:62]([OH:68])=[O:63].[NH2:35][CH:36]([CH2:40][C:41]1[CH:42]=[CH:43][C:44]([C:47]#[N:48])=[CH:45][CH:46]=1)[C:37]([N:10]1[CH2:11][CH2:16][CH2:15][CH2:14]1)=[O:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6422Trifluoroacetic acidHCID 7525EthylmorpholineHCID 31268PyrrolidineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 43933462-Tert-butoxycarbonylamino-3-(4-cyano-phenyl)-propionic acid

生成物 1

HCID 23002643HCID 23002643、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

7.5 g of BOP are added to a mixture of 4.06 g of 2-(tert-butoxycarbonylamino)-3-(4-cyanophenyl)propionic acid and 1.15 ml of pyrrolidine in 20 ml of DMF, and the mixture is stirred for 2 hours at RT, while keeping the pH at 7 by adding N-ethylmorpholine. The reaction mixture is concentrated under vacuum and the residue is chromatographed on silica gel, eluting with a chloroform/MeOH mixture (95/5; v/v). The product obtained is taken up in 20 ml of TFA in 20 ml of DCM, and the reaction mixture is stirred for 30 minutes at RT and concentrated under vacuum. The residue is taken up in ether and the precipitate formed is filtered off by suction. 3.95 g of the expected product are obtained after drying.

後処理

  1. concentrationThe reaction mixture is concentrated under vacuum
  2. customthe residue is chromatographed on silica gel
  3. washeluting with a chloroform/MeOH mixture (95/5; v/v)
  4. customThe product obtained
  5. stirringthe reaction mixture is stirred for 30 minutes at RT
  6. concentrationconcentrated under vacuum
  7. customthe precipitate formed
  8. filtrationis filtered off by suction

出典と根拠

ORDレコード
ord-da0a9db19de74e02886b0026c8a0cdb5
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07157454B2

反応ノート

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