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Potassium Carbonate → (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-1-(4-dimethylamino-piperidin-1-yl)-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butan-1,4-dione

HRID 736942
ノート
印刷プレビュー

反応式

HRID 736942 の反応式
CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(C(C)C)C(C)C)C.[CH3:32][N:33]([CH3:40])[CH:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1.[NH2:41][C:42]1[C:73]([C:74]([F:77])([F:76])[F:75])=[CH:72][C:45]([CH2:46][C@@H:47]([CH2:51][C:52](=[O:71])[N:53]2[CH2:58][CH2:57][CH:56]([N:59]3[CH2:65][CH2:64][C:63]4[CH:66]=[CH:67][CH:68]=[CH:69][C:62]=4[NH:61][C:60]3=[O:70])[CH2:55][CH2:54]2)[C:48](O)=[O:49])=[CH:44][C:43]=1[Cl:78].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[NH2:41][C:42]1[C:73]([C:74]([F:76])([F:75])[F:77])=[CH:72][C:45]([CH2:46][C@@H:47]([CH2:51][C:52]([N:53]2[CH2:58][CH2:57][CH:56]([N:59]3[CH2:65][CH2:64][C:63]4[CH:66]=[CH:67][CH:68]=[CH:69][C:62]=4[NH:61][C:60]3=[O:70])[CH2:55][CH2:54]2)=[O:71])[C:48]([N:37]2[CH2:38][CH2:39][CH:34]([N:33]([CH3:40])[CH3:32])[CH2:35][CH2:36]2)=[O:49])=[CH:44][C:43]=1[Cl:78]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 417391N,N-Dimethylpiperidin-4-amineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 68591515(S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butanoic acid

生成物 1

HCID 57848212
(S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-1-(4-dimethylamino-piperidin-1-yl)-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butan-1,4-dione

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

80.3 mg (0.25 mmol) TBTU, 0.21 mL (1.2 mmol) ethyldiisopropylamine and 38.5 mg (0.3 mmol) dimethyl-piperidin-4-yl-amine were added to a solution of 130 mg (0.24 mmol) (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butanoic acid in 10 mL DMF and the reaction mixture was stirred overnight at RT. The reaction solution was poured into 80 mL 15% K2CO3 solution, stirred for 10 min at RT, the precipitated substance was suction filtered, washed with 5 mL water and dried in the air over the weekend. Then the product was purified by chromatography using HPLC.

後処理

  1. stirringstirred for 10 min at RT
  2. filtrationfiltered
  3. washwashed with 5 mL water
  4. customdried in the air over the weekend
  5. customThen the product was purified by chromatography

出典と根拠

ORDレコード
ord-4ed3dbde9fc544ffa4d97abd5cb99b99
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07595312B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート