Diisopropylethylamine → HCID 58017568、化合物

HRID 1694376

反応式

HRID 1694376 の反応式
C(OC([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[C:17]([OH:19])=O)[CH2:10][CH2:9]1)=O)(C)(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:44][C:45]1([C:48]2[CH:57]=[CH:56][C:51]([C:52]([O:54][CH3:55])=[O:53])=[CH:50][CH:49]=2)[CH2:47][CH2:46]1.CCN(C(C)C)C(C)C.C([O-])(O)=O.[Na+]>C(#N)C>[NH:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[C:17]([NH:44][C:45]2([C:48]3[CH:57]=[CH:56][C:51]([C:52]([O:54][CH3:55])=[O:53])=[CH:50][CH:49]=3)[CH2:47][CH2:46]2)=[O:19])[CH2:10][CH2:9]1

参加物

7

反応物 5

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 14977845N-Boc-indoline-7-carboxylic acidHCID 45140209Methyl 4-(1-aminocyclopropyl)benzoate

生成物 1

HCID 58017568HCID 58017568、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-(tert-butoxycarbonyl)indoline-7-carboxylic acid (300 mg, 1.14 mmol), HATU (475 mg, 21.2 mmol) and methyl 4-(1-aminocyclopropyl)benzoate (262 mg, 1.37 mmol) were added to acetonitrile (7.6 ml). The solution was cooled in an ice bath and DIPEA (695 ul, 3.99 mmol) was added. After 2 hr at RT, the mixture was poured into a solution of NaHCO3 (½ sat.) and washed 3 times with EtOAc. The combined organic layers were washed with brine and dried with Na2SO4. The solvent was removed and the crude mixture purified by flash chromatography on silica gel. The Boc group was removed with 1:1 TFA/DCM using the standard procedure.

後処理

  1. temperatureThe solution was cooled in an ice bath
  2. washwashed 3 times with EtOAc
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried with Na2SO4
  5. customThe solvent was removed
  6. customthe crude mixture purified by flash chromatography on silica gel
  7. customThe Boc group was removed with 1:1 TFA/DCM using the standard procedure

出典と根拠

ORDレコード
ord-6ccbfe3566654562ad5557ca8317821b
出典データセット
uspto-grants-2012_04
特許番号
US08158671B2

関連ノート

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