Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 21070238、化合物

HRID 1371541

反応式

HRID 1371541 の反応式
[C:1]([NH:8][C@H:9]([C:19]([OH:21])=O)[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].CN([C:25]([O:29][N:30]1N=NC2C=CC=C[C:31]1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C.Cl.CNOC>C(Cl)Cl>[C:1]([NH:8][CH:9]([CH2:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]#[N:18])=[CH:15][CH:16]=1)[C:19]([N:30]([O:29][CH3:25])[CH3:31])=[O:21])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]

参加物

6

反応物 4

HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 7020841N-(tert-Butoxycarbonyl)-4-cyano-L-phenylalanine

生成物 1

HCID 21070238HCID 21070238、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2 g of (N-Boc)-4-cyanophenylalanine, 2.32 g of TBTU, 2.40 ml of DIPEA and 806 mg of N,O-dimethylhydroxylamine hydrochloride are mixed together in 30 ml of DCM. After stirring for 24 hours at RT, the reaction mixture is concentrated to dryness and the residue is then extracted with EtOAc. The organic phase is washed with a pH 2 buffer solution, a saturated NaHCO3 solution and then a saturated NaCl solution. The expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g).

後処理

  1. concentrationthe reaction mixture is concentrated to dryness
  2. extractionthe residue is then extracted with EtOAc
  3. washThe organic phase is washed with a pH 2 buffer solution
  4. customThe expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g)

出典と根拠

ORDレコード
ord-90a6d7c751cc4148b1a4a3cdbb4e6014
出典データセット
uspto-grants-2007_01
特許番号
US07157454B2

関連ノート

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