HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Water → HCID 21471776, compound

HRID 1734064
Notes
Print preview

Reaction equation

HRID 1734064 reaction equation
[Cl:1][CH2:2][C:3]([C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1)=O.O>C([SiH](CC)CC)C.FC(F)(F)C(O)=O>[Cl:1][CH2:2][CH2:3][C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 962WaterHCID 21472076HCID 21472076, compound

Product 1

HCID 21471776HCID 21471776, compoundYield 47.5%

Reagents, catalysts & solvents 2

HCID 6422Trifluoroacetic acidSolventHCID 12052TriethylsilaneSolvent

Conditions

Temperature
50 °C

Procedure

A mixture of 1.9 g of 2-chloroacetyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one in 5.4 ml of triethylsilane and 15 ml of trifluoroacetic acid was stirred at 50° C. for 12 hours. The mixture was poured into water, alkalified and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by column chromatography on a silica gel to give 0.85 g of 2-chloroethyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one as white crystals, m.p. 156°-158° C.

Workup

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography on a silica gel

Sources & evidence

ORD record
ord-4d15ec676cfb411ea4a37f98e9ecc9d9
Source dataset
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05532240

Reaction notes

Loading…

On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes