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HCID 71256713, compound → HCID 71256586, compound

HRID 1627730
Notes
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Reaction equation

HRID 1627730 reaction equation
[C:1]([C:3]1[S:4][C:5]2[CH:11]=[C:10]([O-:12])[CH:9]=[CH:8][C:6]=2[N:7]=1)#[N:2].C([N+](CCCC)(CCCC)CCCC)CCC.I[CH2:31]/[CH:32]=[CH:33]/[B:34]1[O:38][C:37]([CH3:40])([CH3:39])[C:36]([CH3:42])([CH3:41])[O:35]1>ClCCl>[CH3:39][C:37]1([CH3:40])[C:36]([CH3:41])([CH3:42])[O:35][B:34](/[CH:33]=[CH:32]/[CH2:31][O:12][C:10]2[CH:9]=[CH:8][C:6]3[N:7]=[C:3]([C:1]#[N:2])[S:4][C:5]=3[CH:11]=2)[O:38]1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 71256713HCID 71256713, compoundHCID 86676860(E)-2-(3-iodoprop-1-en-1-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

Product 1

HCID 71256586HCID 71256586, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
80 °C

Procedure

A reaction vial was charged with tetrabutylammonium 2-cyanobenzo[d]thiazol-6-olate (209 mg, 1.19 mmol), (E)-2-(3-iodoprop-1-en-1-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (386 mg, 1.31 mmol) and 15 mL of dry dichloromethane. The vial was sealed, and the solution was heated in an oil bath at 80° C. overnight (˜16 hours). The crude reaction mixture was added to 1 gram of celite, and the solvent was evaporated under vacuum. The product was purified by silica gel chromatography using an increasing gradient of ethyl acetate in dichloromethane as eluent. This gave 166 mg of (E)-6-((3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)allyl)oxy)benzo[d]thiazole-2-carbonitrile as a colorless oil that crystallized to a white solid upon standing at ambient temperature.

Workup

  1. customA reaction
  2. customThe vial was sealed
  3. customThe crude reaction mixture
  4. additionwas added to 1 gram of celite
  5. customthe solvent was evaporated under vacuum
  6. customThe product was purified by silica gel chromatography
  7. customThis gave 166 mg of (E)-6-((3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)allyl)oxy)benzo[d]thiazole-2-carbonitrile as a colorless oil that crystallized to a white solid
  8. customupon standing at ambient temperature

Sources & evidence

ORD record
ord-f3416c70632a4083a849de65f7fd4e7e
Source dataset
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08785652B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes