3-Amino-1,2-propanediol → HCID 14700208, 화합물

HRID 1651511노트

반응식

HRID 1651511 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 14700208HCID 14700208, 화합물수율 72.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d9fc4a3d30a4aed8c45720ed3f55aad
출처 데이터셋
uspto-grants-1990_05
특허 번호
US04929549

반응 노트

불러오는 중…