Formaldehyde → (S)-4-(2-chloro-7-methyl-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-yl)-3-methylmorpholine

HRID 1626575ノート

反応式

HRID 1626575 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][C@@H:16]2[CH3:21])[C:5]2[CH2:10][N:9]([CH2:11][CH:12]3CC3)[CH2:8][C:6]=2[N:7]=1.C=O.Cl.ClC1N=C(N2CCOC[C@@H]2C)C2CCNCC=2N=1>>[Cl:1][C:2]1[N:3]=[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][C@@H:16]2[CH3:21])[C:5]2[CH2:12][CH2:11][N:9]([CH3:10])[CH2:8][C:6]=2[N:7]=1

参加物

4

反応物 3

HCID 712FormaldehydeHCID 86663153(S)-4-(2-chloro-6-(cyclopropylmethyl)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-4-yl)-3-methylmorpholineHCID 86663157(S)-4-(2-chloro-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-yl)-3-methylmorpholine hydrochloride

生成物 1

HCID 86663156(S)-4-(2-chloro-7-methyl-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-yl)-3-methylmorpholine収率 78%

実験手順

Method as described for intermediate 8 using formaldehyde (37% solution in water) and (S)-4-(2-chloro-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-yl)-3-methylmorpholine hydrochloride as starting materials. The mixture was partitioned between saturated NaHCO3 solution and DCM. The organic layer was recovered, dried over MgSO4, filtered and reduced in vacuo, yielding the title compound (2.11 g, 7.47 mmol, 78%).

後処理

  1. customThe mixture was partitioned between saturated NaHCO3 solution and DCM
  2. customThe organic layer was recovered
  3. dry with materialdried over MgSO4
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-4ddc060b4eca455c9fc74846fd6ef09b
出典データセット
uspto-grants-2014_07
特許番号
US08785457B2

反応ノート

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