Benzylamine → HCID 19805433、化合物

HRID 631886

反応式

HRID 631886 の反応式
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:5]=1[C:6]([OH:8])=O)([O-:3])=[O:2].[CH2:14]([NH2:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN1C(=O)CCC1.CCN(C(C)C)C(C)C.C(OCC)(=O)C>[CH2:14]([NH:21][C:6](=[O:8])[C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:13])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

7

反応物 3

HCID 7504BenzylamineHCID 160976-Methyl-2-nitrobenzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 19805433HCID 19805433、化合物収率 75.5%

試薬・触媒・溶媒 3

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒HCID 81531Diisopropylethylamine溶媒

実験手順

2-Nitro-6-methylbenzoic acid (0.91 g) and benzylamine (0.53 g) were dissolved in NMP (5 mL) and DIPEA (3 mL). HATU (1.9 g) was added and the mixture was stirred for 1 hour. The reaction mixture was diluted with ethyl acetate and washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate and then brine. The organic solution was dried with magnesium sulfate, filtered and the solvent was removed under vacuum to give a light brown oil (1.01 g) that crystallized on standing.

後処理

  1. washwashed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate
  2. dry with materialThe organic solution was dried with magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-1218be025e15465492c80ea8cb1c6832
出典データセット
uspto-grants-2016_04
特許番号
US09321740B2

関連ノート

読み込み中…