Trifluoroacetic acid → 7-(7H-Pyrrolo[2,3-d]pyrimidin-4-yl)-4,7-diaza-spiro[2.5]octane-4-sulfonic acid bis-(3-cyano-propyl)-amide

HRID 589973ノート

反応式

HRID 589973 の反応式
C(OC([N:8]1[C:12]2[N:13]=[CH:14][N:15]=[C:16]([N:17]3[CH2:24][C:21]4([CH2:23][CH2:22]4)[N:20]([S:25](=[O:38])(=[O:37])[N:26]([CH2:32][CH2:33][CH2:34][C:35]#[N:36])[CH2:27][CH2:28][CH2:29][C:30]#[N:31])[CH2:19][CH2:18]3)[C:11]=2[CH:10]=[CH:9]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C1COCC1>[C:30]([CH2:29][CH2:28][CH2:27][N:26]([CH2:32][CH2:33][CH2:34][C:35]#[N:36])[S:25]([N:20]1[CH2:19][CH2:18][N:17]([C:16]2[C:11]3[CH:10]=[CH:9][NH:8][C:12]=3[N:13]=[CH:14][N:15]=2)[CH2:24][C:21]21[CH2:23][CH2:22]2)(=[O:38])=[O:37])#[N:31]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 682960054-{4-[Bis-(3-cyano-propyl)-sulfamoyl]-4,7-diaza-spiro[2.5]oct-7-yl}-pyrrolo[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester2 回

生成物 1

HCID 574106987-(7H-Pyrrolo[2,3-d]pyrimidin-4-yl)-4,7-diaza-spiro[2.5]octane-4-sulfonic acid bis-(3-cyano-propyl)-amide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4-{4-[Bis-(3-cyano-propyl)-sulfamoyl]-4,7-diaza-spiro[2.5]oct-7-yl}-pyrrolo[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester (intermediate 19) was dissolved in THF (1 mL), added TFA (0.5 mL) and then stirred at rt for 2 h. The crude reaction mixture was concentrated in vacuo and redissolved in MeOH (0.5 mL). The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

後処理

  1. customThe crude reaction mixture
  2. concentrationwas concentrated in vacuo
  3. dissolutionredissolved in MeOH (0.5 mL)
  4. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture

出典と根拠

ORDレコード
ord-4037e1dfea054296a53ef464999180dc
出典データセット
uspto-grants-2016_01
特許番号
US09233964B2

反応ノート

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