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2-Furanmethanaminium, N,N,N-trimethyl-, iodide (1:1) → HCID 21520115、化合物

HRID 1605523
ノート
印刷プレビュー

反応式

HRID 1605523 の反応式
[SH:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([S:18](=[O:21])(=[O:20])[NH2:19])[C:10]=1[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:5]([OH:7])=[O:6].C(=O)([O-])[O-].[K+].[K+].[I-].C[N+](C)(C)[CH2:31][C:32]1[O:36][CH:35]=[CH:34][CH:33]=1.[OH-].[Na+]>C(OCCOCCOCC)C>[O:36]1[CH:35]=[CH:34][CH:33]=[C:32]1[CH2:31][S:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([S:18](=[O:21])(=[O:20])[NH2:19])[C:10]=1[O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:5]([OH:7])=[O:6]
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

6

反応物 4

HCID 109372-Furanmethanaminium, N,N,N-trimethyl-, iodide (1:1)HCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 21520079HCID 21520079、化合物

生成物 1

HCID 21520115HCID 21520115、化合物

試薬・触媒・溶媒 1

HCID 8179Diethylene glycol diethyl ether
溶媒

反応条件

温度
110 °C

実験手順

To a solution of 3-mercapto-4-phenoxy-5-sulfamylbenzoic acid (1.6 g) in diethylene glycol diethyl ether (15 ml), anhydrous potassium carbonate (0.5 g) and trimethylfurfurylammonium iodide (2 g) were added. The resulting mixture is stirred at 110° C. for 4 hours, cooled and poured into 0.3 N sodium hydroxide (75 ml). After extraction twice with diethyl ether, the aqueous layer is adjusted to pH 3 by addition of acetic acid. The reaction product is extracted with ethyl acetate, and the resulting organic solution is evaporated in vacuo. The residue is triturated with aqueous acetone giving rise to crystallisation. The 3-(2-furylmethylthio)-4-phenoxy-5-sulfamylbenzoic acid thus obtained is recrystallized from aqueous ethanol and dried. The compound is obtained with a melting point of 214°-216° C.

後処理

  1. temperaturecooled
  2. extractionAfter extraction twice with diethyl ether
  3. additionthe aqueous layer is adjusted to pH 3 by addition of acetic acid
  4. extractionThe reaction product is extracted with ethyl acetate
  5. customthe resulting organic solution is evaporated in vacuo
  6. customThe residue is triturated with aqueous acetone giving rise to crystallisation

出典と根拠

ORDレコード
ord-d67c2457057a4adb895b7e713365ef3d
出典データセット
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03950376

反応ノート

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