3,3,3-Trifluoropropylamine → HCID 71290300、化合物

HRID 536509ノート

反応式

HRID 536509 の反応式
[F:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[CH2:4][N:5]1[C:9]2[CH2:10][CH2:11][CH2:12][C:8]=2[C:7]([C:13]2[N:14]=[C:15](I)[C:16]3[C:21]([CH3:23])([CH3:22])[C:20](=[O:24])[NH:19][C:17]=3[N:18]=2)=[N:6]1.[F:30][C:31]([F:36])([F:35])[CH2:32][CH2:33][NH2:34]>CN1C(=O)CCC1>[F:1][C:2]1[CH:29]=[CH:28][CH:27]=[CH:26][C:3]=1[CH2:4][N:5]1[C:9]2[CH2:10][CH2:11][CH2:12][C:8]=2[C:7]([C:13]2[N:14]=[C:15]([NH:34][CH2:33][CH2:32][C:31]([F:36])([F:35])[F:30])[C:16]3[C:21]([CH3:23])([CH3:22])[C:20](=[O:24])[NH:19][C:17]=3[N:18]=2)=[N:6]1

参加物

4

反応物 2

HCID 100013,3,3-TrifluoropropylamineHCID 71746453HCID 71746453、化合物

生成物 1

HCID 71290300HCID 71290300、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
150 °C

実験手順

40 mg (0.07 mmol) of 2-[1-(2-fluorobenzyl)-1,4,5,6-tetrahydrocyclopenta[c]pyrazol-3-yl]-4-iodo-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one (example 33A) was dissolved in 1 ml of absolute NMP and 334 mg (2.96 mmol) of 3,3,3-trifluoropropan-1-amine was added. The mixture was heated in the microwave for 2 h at 150° C. and 1 h at 150° C. The reaction solution was filtered and purified by preparative HPLC (eluent: acetonitrile/water with 0.1% hydrochloric acid, gradient 20:80→100:0). 27 mg (purity 93%, 70% of theor.) of the target compound was obtained.

後処理

  1. filtrationThe reaction solution was filtered
  2. custompurified by preparative HPLC (eluent: acetonitrile/water with 0.1% hydrochloric acid, gradient 20:80→100:0)
  3. custom27 mg (purity 93%, 70% of theor.) of the target compound was obtained

出典と根拠

ORDレコード
ord-6b42ff5f1b05426397e15717935b49b3
出典データセット
uspto-grants-2014_10
特許番号
US08859569B2

反応ノート

読み込み中…