Toluene → HCID 15085579、化合物

HRID 1607523ノート

反応式

HRID 1607523 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[NH2:10])=[O:4].[CH2:11]([N:13]([CH2:16]C)CC)C.C(Cl)(Cl)=[O:19].C1(C)C=CC=CC=1>O1CCCC1>[CH3:11][NH:13][C:16](=[O:19])[NH:10][C:9]1[CH:8]=[CH:7][S:6][C:5]=1[C:3]([O:2][CH3:1])=[O:4]

参加物

6

反応物 4

HCID 1140TolueneHCID 6371PhosgeneHCID 8471TriethylamineHCID 89652Methyl 3-amino-2-thiophenecarboxylate

生成物 1

HCID 15085579HCID 15085579、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of methyl-3-amino-thiophene-2-carboxylate (5 g, 31,8 mmole) and triethylamine (4,43 ml, 31,8 mmole) in dry tetrahydrofuran (100 ml) was added dropwise a 20% phosgene solution in toluene (31,8 mmole). After the addition had been completed the mixture was heated to reflux for 30 min, followed by filtration at room temperature. The filtrate was evaporated in vacuo, whereafter the crystalline residue was suspended in water (200 ml). Filtration of the suspension left the title compound as white crystals. M.p. 141°-142° C.

後処理

  1. additionAfter the addition
  2. temperaturewas heated
  3. temperatureto reflux for 30 min
  4. filtrationfollowed by filtration at room temperature
  5. customThe filtrate was evaporated in vacuo, whereafter the crystalline residue
  6. filtrationFiltration of the suspension
  7. waitleft the title compound as white crystals

出典と根拠

ORDレコード
ord-416f9324956a49c688a00cd94c5dbc9e
出典データセット
uspto-grants-1989_09
特許番号
US04866065

反応ノート

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