Phosphoric Acid → 2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol monophosphate

HRID 1398231

反応式

HRID 1398231 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([C:9]2[N:13]3[CH2:14][CH2:15][CH2:16][C@@:17]([C:28]([OH:31])([CH3:30])[CH3:29])([O:18][C:19]4[CH:24]=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[CH:20]=4)[C:12]3=[N:11][N:10]=2)[CH:6]=[CH:5][C:4]=1[N:32]1[CH:36]=[C:35]([CH3:37])[N:34]=[CH:33]1.[P:38](=O)([OH:41])([OH:40])[OH:39]>CC(O)C>[P:38]([O:31][C:28]([C@@:17]1([O:18][C:19]2[CH:24]=[C:23]([F:25])[C:22]([F:26])=[C:21]([F:27])[CH:20]=2)[CH2:16][CH2:15][CH2:14][N:13]2[C:9]([C:7]3[CH:6]=[CH:5][C:4]([N:32]4[CH:36]=[C:35]([CH3:37])[N:34]=[CH:33]4)=[C:3]([O:2][CH3:1])[N:8]=3)=[N:10][N:11]=[C:12]12)([CH3:30])[CH3:29])([OH:41])([OH:40])=[O:39]

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 569296452-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol

生成物 1

HCID 666076052-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol monophosphate収率 93.5%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

To a mixture of 2-{(8R)-3-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]-8-(3,4,5-trifluorophenoxy)-5,6,7,8-tetrahydro[1,2,4]triazolo[4,3-a]pyridin-8-yl}propan-2-ol (1.0 g) in 2-propanol (4 mL) was added a mixture of phosphoric acid (0.27 g) in 2-propanol (2 mL) at 50° C., and the mixture was stirred for 30 min. To the reaction mixture was added IPE (6 mL) at 50° C., and the mixture was stirred for 30 min. To the reaction mixture was added IPE (2 mL) at room temperature, and the mixture was stirred for 30 min. The crystals were collected by filtration, washed with IPE (2 mL) and dried to give the title compound (1.08 g).

後処理

  1. additionwas added
  2. additionTo the reaction mixture was added IPE (6 mL) at 50° C.
  3. stirringthe mixture was stirred for 30 min
  4. additionTo the reaction mixture was added IPE (2 mL) at room temperature
  5. stirringthe mixture was stirred for 30 min
  6. filtrationThe crystals were collected by filtration
  7. washwashed with IPE (2 mL)
  8. customdried

出典と根拠

ORDレコード
ord-8b15fed96e6847208e4d138e79d5d54a
出典データセット
uspto-grants-2014_12
特許番号
US08901309B2

関連ノート

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