3-Amino-1,2-propanediol → HCID 14700208、化合物

HRID 1651511ノート

反応式

HRID 1651511 の反応式
CO[C:3]([C:5]1[S:9][C:8]2[S:10][C:11]([S:13]([NH2:16])(=[O:15])=[O:14])=[CH:12][C:7]=2[CH:6]=1)=[O:4].[OH:17][CH:18]([CH2:21][OH:22])[CH2:19][NH2:20]>CO>[OH:17][CH:18]([CH2:21][OH:22])[CH2:19][NH:20][C:3]([C:5]1[S:9][C:8]2[S:10][C:11]([S:13]([NH2:16])(=[O:14])=[O:15])=[CH:12][C:7]=2[CH:6]=1)=[O:4]

参加物

4

反応物 2

HCID 735613-Amino-1,2-propanediolHCID 14700202Methyl 5-sulfamoylthieno[2,3-b]thiophene-2-carboxylate

生成物 1

HCID 14700208HCID 14700208、化合物収率 72.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-Methoxycarbonylthieno[2,3-b]thiophene-2-sulfonamide (0.83 g., 3 mmoles) and 2,3-dihydroxypropylamine (1.37 g., 15 mmoles) were dissolved in hot methanol and refluxed for 48 hours. The reaction was worked up by evaporating the methanol in vacuo. Water (7 mL) was added followed by the dropwise addition of conc. HCl until strongly acidic (~1.8 pH). The product crystallized out and was collected, washed with water and dried to give 0.90 g of crude product. Recrystallization from nitromethane gave 0.73 g of 5-(N-2,3-dihydroxypropylcarbamoyl)thieno[2,3-b]thiophene-2-sulfonamide, m.p. 117°-118° C.

後処理

  1. temperaturerefluxed for 48 hours
  2. customby evaporating the methanol in vacuo
  3. additionWater (7 mL) was added
  4. additionfollowed by the dropwise addition of conc. HCl until strongly acidic (~1.8 pH)
  5. customThe product crystallized out
  6. customwas collected
  7. washwashed with water
  8. customdried
  9. customto give 0.90 g of crude product
  10. customRecrystallization from nitromethane

出典と根拠

ORDレコード
ord-7d9fc4a3d30a4aed8c45720ed3f55aad
出典データセット
uspto-grants-1990_05
特許番号
US04929549

反応ノート

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