Tetra-n-butylammonium di-tert-butylphosphate → [2-[2-Amino-4-(isoindoline-2-carbonyl)quinazolin-6-yl]-4,5-difluorophenyl]methyl di-tert-butyl phosphate

HRID 1631181ノート

反応式

HRID 1631181 の反応式
[C:1]([O:5][P:6]([O-:13])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].C([N+](CCCC)(CCCC)CCCC)CCC.[NH2:31][C:32]1[N:41]=[C:40]([C:42]([N:44]2[CH2:52][C:51]3[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=3)[CH2:45]2)=[O:43])[C:39]2[C:34](=[CH:35][CH:36]=[C:37]([C:53]3[CH:58]=[C:57]([F:59])[C:56]([F:60])=[CH:55][C:54]=3[CH2:61]Cl)[CH:38]=2)[N:33]=1>C(#N)C>[P:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([O:13][CH2:61][C:54]1[CH:55]=[C:56]([F:60])[C:57]([F:59])=[CH:58][C:53]=1[C:37]1[CH:38]=[C:39]2[C:34](=[CH:35][CH:36]=1)[N:33]=[C:32]([NH2:31])[N:41]=[C:40]2[C:42]([N:44]1[CH2:45][C:46]2[C:51](=[CH:50][CH:49]=[CH:48][CH:47]=2)[CH2:52]1)=[O:43])=[O:7]

参加物

4

反応物 2

HCID 22339116Tetra-n-butylammonium di-tert-butylphosphateHCID 66837605[2-Amino-6-(2-chloromethyl-4,5-difluorophenyl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone

生成物 1

HCID 66836649[2-[2-Amino-4-(isoindoline-2-carbonyl)quinazolin-6-yl]-4,5-difluorophenyl]methyl di-tert-butyl phosphate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

800 mg of tetrabutylammonium di-tert-butylphosphate are added to 270 mg of [2-amino-6-(2-chloromethyl-4,5-difluorophenyl)quinazolin-4-yl]-(1,3-dihydroisoindol-2-yl)methanone dissolved in 20 ml of acetonitrile, and the solution obtained is heated at 80° C. for 2 h. After cooling to 25° C., undissolved material is filtered off, and the filtrate is evaporated to dryness in vacuo. The residue is dissolved in 1 ml of dimethyl sulfoxide and purified by chromatography (reversed phase).

後処理

  1. customthe solution obtained
  2. temperatureAfter cooling to 25° C.
  3. filtrationundissolved material is filtered off
  4. customthe filtrate is evaporated to dryness in vacuo
  5. dissolutionThe residue is dissolved in 1 ml of dimethyl sulfoxide
  6. custompurified by chromatography (reversed phase)

出典と根拠

ORDレコード
ord-44a1641c3abb4f5384e7ba77deb27cf0
出典データセット
uspto-grants-2014_07
特許番号
US08791129B2

反応ノート

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