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Water → Tert. butyl 6-[4-(7-methoxy-2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-5-methyl-pyrimidin-4-carboxylate

HRID 74553
ノート
印刷プレビュー

反応式

HRID 74553 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1.CCN(C(C)C)C(C)C.Cl[C:31]1[N:36]=[CH:35][N:34]=[C:33]([C:37]([O:39][C:40]([CH3:43])([CH3:42])[CH3:41])=[O:38])[C:32]=1[CH3:44].O>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][N:17]([C:31]4[N:36]=[CH:35][N:34]=[C:33]([C:37]([O:39][C:40]([CH3:42])([CH3:41])[CH3:43])=[O:38])[C:32]=4[CH3:44])[CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 58386606Tert. butyl 6-chloro-5-methyl-pyrimidine-4-carboxylate

生成物 1

HCID 58386534Tert. butyl 6-[4-(7-methoxy-2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-5-methyl-pyrimidin-4-carboxylate

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

0.20 g (0.73 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 0.14 mL (0.80 mmol) DIPEA were placed in 3.0 mL DMF. 0.17 g (0.74 mmol) tert. butyl 6-chloro-5-methyl-pyrimidine-4-carboxylate were added and the reaction mixture was stirred for 3 h at RT. The reaction mixture was mixed with water and extracted with DCM. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was combined with diisopropylether and the precipitated solid was suction filtered and dried.

後処理

  1. extractionextracted with DCM
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. concentrationconcentrated to dryness by rotary evaporation
  5. filtrationfiltered
  6. customdried

出典と根拠

ORDレコード
ord-f498d6096553424e9a7627d278a1d9ee
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829006B2

反応ノート

読み込み中…

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