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Trifluoroacetic acid → HCID 23002643、化合物

HRID 850005
ノート
印刷プレビュー

反応式

HRID 850005 の反応式
C([NH:8][CH:9]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]#[N:21])=[CH:16][CH:15]=1)[C:10]([OH:12])=O)(OC(C)(C)C)=O.[NH:22]1[CH2:26][CH2:25][CH2:24][CH2:23]1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.[C:54]([OH:60])([C:56]([F:59])([F:58])[F:57])=[O:55]>CN(C=O)C.C(Cl)Cl.CCN(CC)CC>[F:57][C:56]([F:59])([F:58])[C:54]([OH:60])=[O:55].[NH2:8][CH:9]([CH2:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]#[N:21])=[CH:18][CH:19]=1)[C:10]([N:22]1[CH2:26][CH2:25][CH2:24][CH2:23]1)=[O:12]
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 4

HCID 6422Trifluoroacetic acidHCID 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 3

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒
HCID 8471Triethylamine溶媒

実験手順

4.06 g of 2-[N-(Boc)amino]-3-(4-cyanophenyl)propionic acid are mixed with 1.15 ml of pyrrolidine and 7.5 g of BOP in 20 ml of DMF; the mixture is left stirring for 2 hours at RT while maintaining at pH=7 by addition of Et3N. After evaporating to dryness, the residue is chromatographed on silica, eluting with a chloroform/methanol mixture (9/0.5; v/v). After evaporating off the solvents, the solid obtained is treated with 20 ml of TFA in 20 ml of DCM for 30 minutes at RT. The solvents are evaporated off and the residue is taken up in ether and then dried in order to obtain 3.95 g of the expected product.

後処理

  1. waitthe mixture is left
  2. customAfter evaporating to dryness
  3. customthe residue is chromatographed on silica
  4. washeluting with a chloroform/methanol mixture (9/0.5
  5. customAfter evaporating off the solvents
  6. customthe solid obtained
  7. customThe solvents are evaporated off
  8. customdried in order

出典と根拠

ORDレコード
ord-dc17a0f1f51f4bd58d8b09726df271ff
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06015812

反応ノート

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