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Dimethylformamide → HCID 11668908、化合物

HRID 2244977
ノート
印刷プレビュー

反応式

HRID 2244977 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1NCC(O)=O.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:21]=[O:22])=[CH:16][CH:15]=1.Cl.C([N:31]1[CH2:36][CH2:35][CH2:34][CH2:33][CH:32]1CN)(OC(C)(C)C)=O.F[P-](F)(F)(F)(F)F.[N:46]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:50]2C=CC=CC=2N=N1.[CH3:66][N:67]([CH:69]=[O:70])C>O.CCOC(C)=O>[NH:31]1[CH2:32][CH2:33][CH:34]([CH2:66][NH:67][C:69](=[O:70])[CH:50]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])[NH:46][C:21]([NH:20][C:17]2[CH:18]=[CH:19][C:14]([Cl:13])=[CH:15][CH:16]=2)=[O:22])[CH2:35][CH2:36]1
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 6228Dimethylformamide2 回HCID 76934-Chlorophenyl IsocyanateHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 5171030N-o-FluorophenylglycineHCID 45072188tert-Butyl 2-(aminomethyl)piperidine-1-carboxylate--hydrogen chloride (1/1)

生成物 1

HCID 11668908
HCID 11668908、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-fluorophenylglycine (59 mg, 0.35 mmol) in DMF (4 mL), 4-chlorophenylisocyanate (54 mg, 0.35 mmol) was added. The mixture was stirred at room temperature overnight. To the solution, a solution of N-BOC-aminomethylpiperidine hydrochloride (105 mg, 0.42 mmol) and TEA (0.150 mL, 1.08 mmol) in DMF (4 mL) was added, followed by addition of BOP (239 mg, 0.54 mmol). The mixture was then stirred at room temperature overnight. EtOAc and H2O were added. The organic layer was separated, dried over Na2SO4, concentrated in vacuo.

後処理

  1. stirringThe mixture was then stirred at room temperature overnight
  2. customThe organic layer was separated
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fef33255059a4f9590e7a6568b4ed735
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07678913B2

反応ノート

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