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2-Aminothiazole → HCID 43119856, compound

HRID 1809331
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Reaction equation

HRID 1809331 reaction equation
C([N:3]1[C:11]2[C:6](=[CH:7][C:8]([S:12](Cl)(=[O:14])=[O:13])=[CH:9][CH:10]=2)[CH2:5][CH2:4]1)=O.[NH2:16][C:17]1[S:18][CH:19]=[CH:20][N:21]=1>N1C=CC=CC=1>[S:18]1[CH:19]=[CH:20][N:21]=[C:17]1[NH:16][S:12]([C:8]1[CH:7]=[C:6]2[C:11](=[CH:10][CH:9]=1)[NH:3][CH2:4][CH2:5]2)(=[O:13])=[O:14]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 21552-AminothiazoleHCID 104219941-formyl-2,3-dihydro-1H-indole-5-sulfonyl chloride

Product 1

HCID 43119856HCID 43119856, compoundYield 62%

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
60 °C

Procedure

A mixture of N-formyl-5-(chlorosulfonyl)indoline (60 g, 0.26 mol) and 2-amino thiazole (25 g, 0.26 mol) in pyridine (250 mL) was heated to 60° C. for 1 hour. The reaction mixture was cooled to room temperature and poured into ice/water. The solid was filtered, co-evaporated with toluene until completely dry and used in the next step without further purification. The crude material was brought to reflux in EtOH/KOH (600 mL, 15-20% KOH). After 2 hours a part of the ethanol was removed in vacuo and the light brown precipitate was filtered and crystallized from ethanol. The sulfonamide (39 g, 62% yield) was isolated with a purity of 90% according to HPLC-MS. 1H-NMR (DMSO-d6) δ 7.33-7.30 (m, 2H), 6.87 (d, J=3.8 Hz, 1H), 6.36-6.34 (m, 2H), 5.80 (s, 1H), 3.42 (dt, J=12.0, 4.3 Hz, 2H), 2.88 (t, J=8.5 Hz, 2H).

Workup

  1. temperatureThe reaction mixture was cooled to room temperature
  2. filtrationThe solid was filtered
  3. customuntil completely dry
  4. customused in the next step without further purification
  5. temperatureto reflux in EtOH/KOH (600 mL, 15-20% KOH)
  6. customAfter 2 hours a part of the ethanol was removed in vacuo
  7. filtrationthe light brown precipitate was filtered
  8. customcrystallized from ethanol

Sources & evidence

ORD record
ord-beb5b506e86d4fa1a9c9488504145cd8
Source dataset
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08362032B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes