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Triethylamine → HCID 131711060、化合物

HRID 2163648
ノート
印刷プレビュー

反応式

HRID 2163648 の反応式
C(N(CC)CC)C.[NH2:8][CH:9]1[C:19](=[O:20])[N:11]2[CH:12]([C:17]#[N:18])[C:13]([CH3:16])([CH3:15])[S:14][C@H:10]12.[CH3:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28](Cl)([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH3:41])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>C(Cl)Cl>[CH3:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[C:28]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[CH3:41])([NH:8][CH:9]1[C:19](=[O:20])[N:11]2[CH:12]([C:17]#[N:18])[C:13]([CH3:15])([CH3:16])[S:14][C@H:10]12)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 22750484HCID 22750484、化合物HCID 70604619HCID 70604619、化合物

生成物 1

HCID 131711060HCID 131711060、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-10 °C

実験手順

Triethylamine (444 mg., 4.4 mmole) is added to a suspension of 6-amino-2,2-dimethyl-3-cyanopenam (468 mg., 2 mmole) in methylene chloride (20 ml.) and the resulting mixture cooled to -10° C. A solution of α,α-di(2-methylphenyl)benzyl chloride (614 mg., 2 mmole) in methylene chloride (12 ml.) is added over a ten minute period and the resulting yellow solution stirred for one hour at -10° C. The cooling bath is removed and the mixture stirred and allowed to warm to room temperature. It is stirred for two hours at room temperature and is then concentrated under reduced pressure to a brown sludge. The sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column) using chloroform as eluent. Fractions (15 ml. each) are collected. Fractions 13-19 are combined and concentrated in vacuo to dryness to give 155 mg. of product as a foam.

後処理

  1. customThe cooling bath is removed
  2. stirringthe mixture stirred
  3. temperatureto warm to room temperature
  4. stirringIt is stirred for two hours at room temperature
  5. concentrationis then concentrated under reduced pressure to a brown sludge
  6. customThe sludge is chromatographed on a silica gel column (70-23- mesh., 380 × 20 mm. column)
  7. customeach) are collected
  8. concentrationconcentrated in vacuo to dryness
  9. customto give 155 mg

出典と根拠

ORDレコード
ord-d85a56c6cace408a91dd511c7d736552
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04136096

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート