Ethanol → HCID 178436644、化合物

HRID 1370285

反応式

HRID 1370285 の反応式
C(O)C.[CH2:4]([C:6]1[CH:26]=[CH:25][C:9]([O:10][C:11]2[C:12]([NH:17][C@H:18]3[CH2:23][CH2:22][C@H:21]([OH:24])[CH2:20][CH2:19]3)=[N:13][CH:14]=[N:15][CH:16]=2)=[CH:8][CH:7]=1)[CH3:5].[Cl:27]C1C(OC2C=CC(CC)=CC=2)=CN=CN=1>C(OCC)(=O)C>[ClH:27].[CH2:4]([C:6]1[CH:26]=[CH:25][C:9]([O:10][C:11]2[C:12]([NH:17][C@H:18]3[CH2:19][CH2:20][C@H:21]([OH:24])[CH2:22][CH2:23]3)=[N:13][CH:14]=[N:15][CH:16]=2)=[CH:8][CH:7]=1)[CH3:5]

参加物

5

反応物 3

HCID 702EthanolHCID 223804814-Chloro-5-(4-ethylphenoxy)pyrimidineHCID 178436643HCID 178436643、化合物

生成物 1

HCID 178436644HCID 178436644、化合物収率 77%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

Science, 230-440 mesh) (13×4 cm column bed) using ethyl acetate as the eluent for the first 1.2 L and then with 5% ethanol in ethyl acetate. The fractions that contained homogeneous product were spin evaporated in vacuo to give a syrup. The pure 5-(4-ethylphenoxy)-4-(trans-4-hydroxycyclohexylamino)pyrimidine was converted to the hydrochloride by the same procedure described in Example 4. The residue was triturated under ethyl acetate to give a white solid which was collected, washed with ethyl acetate and dried in vacuo to give 1.25 g (77% yield) of 5-(4-ethylphenoxy)-4-(trans-4-hydroxycyclohexylamino)pyrimidine hydrochloride as a white solid, mp 245-243° C.

後処理

  1. customwere spin evaporated in vacuo
  2. customto give a syrup
  3. customThe residue was triturated under ethyl acetate
  4. customto give a white solid which
  5. customwas collected
  6. washwashed with ethyl acetate
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-947d7ce97c5a47748fdadb301ac840c4
出典データセット
uspto-grants-2003_06
特許番号
US06583148B1

関連ノート

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