Triethylamine → HCID 45377861、化合物

HRID 421297

反応式

HRID 421297 の反応式
C(N(CC)CC)C.[S:8](Cl)([CH3:11])(=[O:10])=[O:9].[CH2:13]([N:17]1[C:25]([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)=[N:24][C:23]2[C:18]1=[N:19][C:20]([C:38]1[CH:39]=[N:40][C:41]([NH2:44])=[N:42][CH:43]=1)=[N:21][C:22]=2[N:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1)[CH:14]([CH3:16])[CH3:15]>CN1C(=O)CCC1>[CH2:13]([N:17]1[C:25]([N:26]2[CH2:31][CH2:30][N:29]([S:8]([CH3:11])(=[O:10])=[O:9])[CH2:28][CH2:27]2)=[N:24][C:23]2[C:18]1=[N:19][C:20]([C:38]1[CH:43]=[N:42][C:41]([NH2:44])=[N:40][CH:39]=1)=[N:21][C:22]=2[N:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1)[CH:14]([CH3:16])[CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chloride2 回HCID 593335015-(9-Isobutyl-6-morpholino-8-(piperazin-1-yl)-9H-purin-2-yl)pyrimidin-2-amine

生成物 1

HCID 45377861HCID 45377861、化合物収率 51%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

Triethylamine (143 μl) and mesyl chloride (50 μl, 0.63 mmol) were added to 5-(9-isobutyl-6-morpholin-4-yl-8-piperazin-1-yl-9H-purin-2-yl)pyrimidin-2-amine (2 ml of solution of 100 mg of this compound in 1 ml of NMP) and the resulting mixture was stirred for 1 hour. Mesyl chloride (50 μl, 0.63 mmol) was further added, the resulting mixture was stirred for 1 hour, then the reaction mixture was partitioned with ethyl acetate and water, and the organic layer was dried over magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid) to give the title compound (135 mg, 51%) as a pale yellow solid.

後処理

  1. stirringthe resulting mixture was stirred for 1 hour
  2. customthe reaction mixture was partitioned with ethyl acetate and water
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)

出典と根拠

ORDレコード
ord-122a053be12a49d19c490a9d3b62a4fa
出典データセット
uspto-grants-2012_01
特許番号
US08097622B2

関連ノート

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