Triethylamine → Methanesulfonic acid 3-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-prop-2-ynyl ester

HRID 2098675ノート

反応式

HRID 2098675 の反応式
[Cl:1][C:2]1[N:3]=[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)[C:5]2[S:10][C:9]([C:11]#[C:12][CH2:13][OH:14])=[CH:8][C:6]=2[N:7]=1.C(N(CC)CC)C.[CH3:28][S:29](Cl)(=[O:31])=[O:30]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[N:3]=[C:4]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)[C:5]2[S:10][C:9]([C:11]#[C:12][CH2:13][O:14][S:29]([CH3:28])(=[O:31])=[O:30])=[CH:8][C:6]=2[N:7]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 866183933-(2-Chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-prop-2-yn-1-ol

生成物 1

HCID 86618394Methanesulfonic acid 3-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-prop-2-ynyl ester

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To 3-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-prop-2-yn-1-ol (142 mg) in chloroform (10 ml) was added triethylamine (77 μL) and methanesulfonyl chloride (49 μL). Stir at room temperature for 2 hours then partition between chloroform and brine, the combined organics were dried (MgSO4). The solvents were removed in vacuo to yield methanesulfonic acid 3-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-yl)-prop-2-ynyl ester (150 mg).

後処理

  1. customthen partition between chloroform and brine
  2. dry with materialthe combined organics were dried (MgSO4)
  3. customThe solvents were removed in vacuo

出典と根拠

ORDレコード
ord-0631533cd3014571bd702626bd7ee84d
出典データセット
uspto-grants-2013_05
特許番号
US08450315B2

反応ノート

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