Acetic Acid → 3-(3-Chloro-4-methoxy-benzylamino)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine

HRID 1602245

反応式

HRID 1602245 の反応式
[NH2:1][C:2]1[C:10]2[C:5](=[N:6][CH:7]=[N:8][C:9]=2[NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[NH:4][N:3]=1.C(O)(=O)C.[Cl:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][C:31]=1[O:32][CH3:33])[CH:27]=O.[BH3-]C#N.[Na+]>CO.CN1C(=O)N(C)CC1>[Cl:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][C:31]=1[O:32][CH3:33])[CH2:27][NH:1][C:2]1[C:10]2[C:5](=[N:6][CH:7]=[N:8][C:9]=2[NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[NH:4][N:3]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 786193-Chloro-4-methoxybenzaldehydeHCID 5003444Sodium cyanoborohydrideHCID 178509242HCID 178509242、化合物

生成物 1

HCID 196105503-(3-Chloro-4-methoxy-benzylamino)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 66611,3-Dimethyl-2-imidazolidinone溶媒

実験手順

Analogously to Example 21, 1.00 mmol of 3-amino-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine in 26 ml of methanol, 13 ml of DMEU and 3.0 mmol of acetic acid are first reacted with 3-chloro-4-methoxy-benzaldehyde and then reduced with 7.00 mmol of NaCNBH3 (5-7 days). 3-(3-Chloro-4-methoxy-benzylamino)-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine is obtained; m.p. 205-208° C.; HPLC: TRet (Grad20-100)=12.2.

出典と根拠

ORDレコード
ord-9803bff3c783425c808218ddbf3b0f95
出典データセット
uspto-grants-1999_11
特許番号
US05981533

関連ノート

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