Hydrochloric Acid → HCID 131728370、化合物

HRID 2076935ノート

反応式

HRID 2076935 の反応式
O=[C:2]1[CH2:7][O:6][C@H:5]([C:8]2[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=2[F:16])[C@@H:4]([NH:17]C(=O)OCCCC)[CH2:3]1.[F:25][C:26]([F:38])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][NH:34][CH2:33][C:31]=2[N:32]=1.[B][B][B][B][B][B][B][B][B][B].[ClH:49]>CO>[ClH:49].[ClH:49].[F:38][C:26]([F:25])([F:37])[C:27]1[N:28]=[CH:29][C:30]2[CH2:36][CH2:35][N:34]([C@H:2]3[CH2:7][O:6][C@H:5]([C:8]4[CH:13]=[C:12]([F:14])[C:11]([F:15])=[CH:10][C:9]=4[F:16])[C@@H:4]([NH2:17])[CH2:3]3)[CH2:33][C:31]=2[N:32]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 184565172-(Trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidineHCID 131728785HCID 131728785、化合物HCID 178419135HCID 178419135、化合物

生成物 1

HCID 131728370HCID 131728370、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of 45 mg (0.13 mmol) of tent-butyl [(2R,3S)-5-oxo-2-(2,4,5-trifluorophenyl)tetrahydro-2H-pyran-3-yl]carbamate and 27 mg (0.13 mmol) of 2-(trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine in 2.0 mL of dry methanol was added 5.0 mg (0.039 mmol) of decaborane. The reaction mixture was stirred overnight and concentrated in vacuo, then purified by preparative thin layer chromatography using an Analtech® 1000 micron plate (5% methanol/methylene chloride, 1% concentrated ammonium hydroxide) to give the product which was stirred with hydrochloric acid in methanol (1.3M, 4 mL) for 1 h to give the title product. LC/MS 432.93 (M+1).

後処理

  1. concentrationconcentrated in vacuo
  2. custompurified by preparative thin layer chromatography
  3. customto give the product which

出典と根拠

ORDレコード
ord-2451d8caf0db4fa782f8aca3f7e5a40d
出典データセット
uspto-grants-2011_04
特許番号
US07928112B2

反応ノート

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