2-Mercaptoethanol → HCID 21564649, compound

HRID 1579971Notes

Reaction equation

HRID 1579971 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH:10]3[S:12][C:7]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)([NH:8][CH2:9]3)[C:6]=2[CH:19]=1.S[CH2:21][CH2:22][OH:23]>C1COCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][CH:10]([S:12][CH2:21][CH2:22][OH:23])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:19]=1

Participants

4

Reactant 2

HCID 15672-MercaptoethanolHCID 21564648HCID 21564648, compound

Product 1

HCID 21564649HCID 21564649, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

A solution of 7-chloro-2,3,4,5-tetrahydro-5-phenyl-2,5-epithio-1H-1,4-benzodiazepine (1g. ) and 2-mercaptoethanol (1 ml) in THF (15 ml) was heated under reflux overnight. The resulting solution was concentrated under reduced pressure and then diluted with ether to induce crystallization of the product. The product was filtered out and washed with ether to give the above-named compound, m.p. 135°-140° (dec.).

Workup

  1. temperatureunder reflux overnight
  2. concentrationThe resulting solution was concentrated under reduced pressure
  3. additiondiluted with ether
  4. customcrystallization of the product
  5. filtrationThe product was filtered out
  6. washwashed with ether
  7. customto give the above-named compound, m.p. 135°-140° (dec.)

Sources & evidence

ORD record
ord-b002c89d97c04203b3524a62b910a6a0
Source dataset
uspto-grants-1976_01
Patent number
US03932399

Reaction notes

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