Water → HCID 16117743、化合物

HRID 2039723ノート

反応式

HRID 2039723 の反応式
Cl.[N:2]1[C:7]2[NH:8][CH:9]=[C:10]([C:11]3[N:16]=[C:15]([C:17]4[CH2:18][CH2:19][NH:20][CH2:21][CH:22]=4)[CH:14]=[CH:13][CH:12]=3)[C:6]=2[CH:5]=[N:4][CH:3]=1.[C:23]([CH2:25][C:26](ON1CCCC1)=[O:27])#[N:24].C(N(C(C)C)CC)(C)C.O>C(O)C>[O:27]=[C:26]([N:20]1[CH2:19][CH:18]=[C:17]([C:15]2[CH:14]=[CH:13][CH:12]=[C:11]([C:10]3[C:6]4[CH:5]=[N:4][CH:3]=[N:2][C:7]=4[NH:8][CH:9]=3)[N:16]=2)[CH2:22][CH2:21]1)[CH2:25][C:23]#[N:24]

参加物

6

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 570164291-Pyrrolidinyl 2-cyanoacetateHCID 69513664HCID 69513664、化合物

生成物 1

HCID 16117743HCID 16117743、化合物収率 16.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

As shown in FIG. 7—step v, compound 29 (30 mg) and 2-cyano acetic acid, pyrrolidin-1-yl ester (47 mg) were mixed in ethanol (2 mL) and diisopropylethylamine (0.084 mL) was added. After stirring at rt for 12 hours, water (30 mL) was added. Extraction with dichloromethane (3×) and chromatographic purification (SiO2, ethyl acetate) afforded 5.3 mg of 3-oxo-3-[6-(7H-pyrrolo[2,3-d]pyrimidin-5-yl)-3′,6′-dihydro-2′H-[2,4′]bipyridinyl-1′-yl]-propionitrile (compound 30).

後処理

  1. extractionExtraction
  2. customwith dichloromethane (3×) and chromatographic purification (SiO2, ethyl acetate)

出典と根拠

ORDレコード
ord-01b70f409264402c960c2992d08ef95a
出典データセット
uspto-grants-2013_11
特許番号
US08580802B2

反応ノート

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