Acetic Acid → HCID 178521048、化合物

HRID 931320ノート

反応式

HRID 931320 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][N:5]([C:7]2([C:10](=[NH:14])OCC)[CH2:9][CH2:8]2)[CH:6]=1.[S].C(O)(=O)C.C(N(CC)CC)C.N[C:28]1[C:33]([NH2:34])=[CH:32][N:31]=[C:30]([N:35]2[CH2:40][CH2:39][O:38][C@@H:37]([C:41]([N:43]3[CH2:47][CH2:46][CH2:45][CH2:44]3)=[O:42])[CH2:36]2)[N:29]=1>>[Cl:1][C:2]1[CH:3]=[N:4][N:5]([C:7]2([C:10]3[NH:14][C:32]4[C:33]([N:34]=3)=[CH:28][N:29]=[C:30]([N:35]3[CH2:40][CH2:39][O:38][C@@H:37]([C:41]([N:43]5[CH2:47][CH2:46][CH2:45][CH2:44]5)=[O:42])[CH2:36]3)[N:31]=4)[CH2:8][CH2:9]2)[CH:6]=1

参加物

6

反応物 5

HCID 176Acetic AcidHCID 8471TriethylamineHCID 5362487SulfurHCID 89853939(R)-(4-(4,5-Diaminopyrimidin-2-yl)morpholin-2-yl)(pyrrolidin-1-yl)methanoneHCID 117966385ethyl 1-(4-chloro-1H-pyrazol-1-yl)cyclopropanecarbimidate

生成物 1

HCID 178521048HCID 178521048、化合物

反応条件

温度
100 °C

実験手順

Ethyl 1-(4-chloro-1H-pyrazol-1-yl)cyclopropanecarbimidate (0.13 g, 0.46 mmol), sulfur (15 mg), acetic acid (0.53 mL, 9.3 mmol) and triethylamine (0.39 mL, 2.79 mmol) were added to the filtrate containing (R)-(4-(4,5-diaminopyrimidin-2-yl)morpholin-2-yl)(pyrrolidin-1-yl)methanone, prepared in the previous step, at room temperature. The reaction mixture was heated to 100° C. for 24 h. The solvent was removed under reduced pressure and the resulting crude material was purified via preparative TLC to afford the title compound (13 mg). MS (ES+APCI) (M+H) 443.0; LCMS retention time 4.485 min (Method T1).

後処理

  1. customprepared in the previous step, at room temperature
  2. customThe solvent was removed under reduced pressure
  3. customthe resulting crude material was purified via preparative TLC

出典と根拠

ORDレコード
ord-0fc590a173bb4398aee2c52c9be96340
出典データセット
uspto-grants-2016_03
特許番号
US09296745B2

反応ノート

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