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Diisopropylethylamine → 6-[4-(7-Methoxy-2-oxo-1,2,4,5-tetrahydro-benzo[d][1,3]diazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylic acidmethoxy-methyl-amide

HRID 469371
ノート
印刷プレビュー

反応式

HRID 469371 の反応式
[CH3:1][O:2][N:3]([CH3:13])[C:4]([C:6]1[CH:11]=[C:10](Cl)[N:9]=[CH:8][N:7]=1)=[O:5].[CH3:14][O:15][C:16]1[CH:17]=[CH:18][C:19]2[NH:25][C:24](=[O:26])[N:23]([CH:27]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)[CH2:22][CH2:21][C:20]=2[CH:33]=1.CCN(C(C)C)C(C)C>C1COCC1.O>[CH3:1][O:2][N:3]([CH3:13])[C:4]([C:6]1[CH:11]=[C:10]([N:30]2[CH2:29][CH2:28][CH:27]([N:23]3[CH2:22][CH2:21][C:20]4[CH:33]=[C:16]([O:15][CH3:14])[CH:17]=[CH:18][C:19]=4[NH:25][C:24]3=[O:26])[CH2:32][CH2:31]2)[N:9]=[CH:8][N:7]=1)=[O:5]
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 3

HCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 581812166-Chloro-pyrimidine-4-carboxylic acidmethoxy-methyl-amide

生成物 1

HCID 581811336-[4-(7-Methoxy-2-oxo-1,2,4,5-tetrahydro-benzo[d][1,3]diazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylic acidmethoxy-methyl-amide

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

0.20 g (0.99 mmol) 6-chloro-pyrimidine-4-carboxylic acidmethoxy-methyl-amide, 0.28 g 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 0.20 mL (1.16 mmol) DIPEA in 1.5 mL THF were heated to 120° C. in the microwave for 30 min. The mixture was diluted with water and extracted with DCM. The combined organic phases were dried on sodium sulphate, filtered and evaporated down i. vac. The residue was triturated with diethyl ether, suction filtered and dried.

後処理

  1. extractionextracted with DCM
  2. customThe combined organic phases were dried on sodium sulphate
  3. filtrationfiltered
  4. customevaporated down i
  5. customThe residue was triturated with diethyl ether, suction
  6. filtrationfiltered
  7. customdried

出典と根拠

ORDレコード
ord-3236cce6c4b142b195a693cfeb07c18e
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629137B2

反応ノート

読み込み中…

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