Pivaloyl chloride → HCID 178447243、化合物

HRID 2289839ノート

反応式

HRID 2289839 の反応式
[NH2:1][C:2]1[NH:7][C:6]2=[N:8][CH:9]=[CH:10][C:5]2=[C:4]([Cl:11])[N:3]=1.[C:12](Cl)(=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14]>N1C=CC=CC=1>[C:12]([NH:1][C:2]1[NH:7][C:6]2=[N:8][CH:9]=[CH:10][C:5]2=[C:4]([Cl:11])[N:3]=1)(=[O:17])[C:13]([CH3:16])([CH3:15])[CH3:14]

参加物

4

反応物 2

HCID 62493Pivaloyl chlorideHCID 178508434HCID 178508434、化合物

生成物 1

HCID 178447243HCID 178447243、化合物収率 83%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-amino-4-chloro-pyrrolo[2,3-d]pyrimidine (20 g, 118 mmol) and pivaloyl chloride (14.3 g, 118 mmol) in pyridine (150 mL) was stirred for 18 hours at ambient temperature. The resulting dark red solution was evaporated to an amber solid which was co-evaporated with water (20 mL, 3×). The resulting solid was filtered, washed with cold water and then dried over KOH in vacuo to yield 22 g (83%) of 2-pivaloylamino-4-chloro-pyrrolo[2,3-d]pyrimidine as a reddish solid. 1H-NMR (DMSO-d6): δ 12.35 (bs, 1, N (7)-H); 10.07 (s,1, N (2)-H); 7.56 (m,1, H-6); 6.58 (m,1, H-5); 1.24 (s, 9, pivaloyl methyls). mp>210° C.

後処理

  1. customThe resulting dark red solution was evaporated to an amber solid which
  2. filtrationThe resulting solid was filtered
  3. washwashed with cold water
  4. dry with materialdried over KOH in vacuo

出典と根拠

ORDレコード
ord-e0f8d61a8926405c9d4cd60ba4e781a0
出典データセット
uspto-grants-2000_07
特許番号
US06093807

反応ノート

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