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Phosgene → HCID 10115938、化合物

HRID 2308505
ノート
印刷プレビュー

反応式

HRID 2308505 の反応式
[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([NH2:12])[S:11][C:7]=2[C:6]([C:13]2[N:14]=[C:15]([C:18]3[CH:19]=[N:20][C:21]([CH3:24])=[CH:22][CH:23]=3)[S:16][CH:17]=2)=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:32](Cl)(Cl)=[O:33].[NH:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1>O1CCOCC1.O>[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([NH:12][C:32]([N:36]3[CH2:41][CH2:40][O:39][CH2:38][CH2:37]3)=[O:33])[S:11][C:7]=2[C:6]([C:13]2[N:14]=[C:15]([C:18]3[CH:19]=[N:20][C:21]([CH3:24])=[CH:22][CH:23]=3)[S:16][CH:17]=2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6371PhosgeneHCID 8083MorpholineHCID 8471TriethylamineHCID 22283166HCID 22283166、化合物

生成物 1

HCID 10115938HCID 10115938、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31275
1,4-Dioxane
溶媒

実験手順

0.1 g of 4-methoxy-7-[2-(6-methyl-pyridin-3-yl)-thiazol-4-yl]-benzothiazol-2-ylamine (0.00028 Mol) were dissolved in dioxane (2 ml) and treated with 0.047 ml triethylamine (0.00034 Mol) and 0.164 ml of phosgene (20% in toluene) (0.00031 Mol). After stirring for 2 hrs. at room temperature 0.122 ml of morpholine (0.0014 Mol) were added and the whole mixture was stirred for 16 hrs. at ambient temperature. Upon addition of water (5 ml) a precipitation formed, which was filtered, washed with water and dried. This crude material was triturated with hot MeOH and after cooling to room temperature filtered. The filtrate was evaporated and the residue subjected to column chromatography (silicagel, CH2Cl2/MeOH+1% NH4OH). The title compound was obtained as a light yellow solid (7%); MS (ISP): m/e=468 (M+H+).

後処理

  1. stirringthe whole mixture was stirred for 16 hrs
  2. customat ambient temperature
  3. customa precipitation
  4. customformed
  5. filtrationwhich was filtered
  6. washwashed with water
  7. customdried
  8. customThis crude material was triturated with hot MeOH
  9. filtrationfiltered
  10. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-436e123706bc497b8a501296a3a2d39b
出典データセット
uspto-grants-2004_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06835732B2

反応ノート

読み込み中…

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