Cyclopropanecarbonyl chloride → HCID 20314164, compound

HRID 2419639Notes

Reaction equation

HRID 2419639 reaction equation
[F:1][C:2]([F:21])([F:20])[C:3]([C:16]([F:19])([F:18])[F:17])([C:5]1[CH:6]=[CH:7][C:8]2[NH:14][CH2:13][CH2:12][CH2:11][CH2:10][C:9]=2[CH:15]=1)[OH:4].[CH:22]1([C:25](Cl)=[O:26])[CH2:24][CH2:23]1>C1(C)C=CC=CC=1>[CH:22]1([C:25]([N:14]2[C:8]3[CH:7]=[CH:6][C:5]([C:3]([C:2]([F:1])([F:20])[F:21])([C:16]([F:19])([F:17])[F:18])[OH:4])=[CH:15][C:9]=3[CH2:10][CH2:11][CH2:12][CH2:13]2)=[O:26])[CH2:24][CH2:23]1

Participants

4

Reactant 2

HCID 77637Cyclopropanecarbonyl chlorideHCID 23346095alpha,alpha-bis(trifluoromethyl)-2,3,4,5-tetrahydro-1H-1-benzazepine-7-methanol

Product 1

HCID 20314164HCID 20314164, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

To 200 ml dry toluene is added 6.3 g (0.020 mole) α,α-bis(trifluoromethyl)-2,3,4,5-tetrahydro-1H-1-benzazepine-7-methanol and 3.0 g (0.025 mole) cyclopropane carboxylic acid chloride. The solution is stirred and heated at reflux under nitrogen for sixteen hours, then cooled and evaporated at reduced pressure. The residual solid is recrystallized from chlorobutane to give 5.0 g, m.p. 165°-167°.

Workup

  1. temperatureheated
  2. temperatureat reflux under nitrogen for sixteen hours
  3. temperaturecooled
  4. customevaporated at reduced pressure
  5. customThe residual solid is recrystallized from chlorobutane
  6. customto give 5.0 g, m.p. 165°-167°

Sources & evidence

ORD record
ord-ed16f582762e42bc9b06fac8ef7463c3
Source dataset
uspto-grants-1978_08
Patent number
US04107303

Reaction notes

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