1-Chloroethyl chloroformate → 5-hydroxy-12-(alpha-chloroethoxycarbonyl)-12H-benzo[a]phenothiazine

HRID 2352225ノート

反応式

HRID 2352225 の反応式
[OH:1][C:2]1[CH:15]=[C:14]2[C:5]([NH:6][C:7]3[C:12]([S:13]2)=[CH:11][CH:10]=[CH:9][CH:8]=3)=[C:4]2[CH:16]=[CH:17][CH:18]=[CH:19][C:3]=12.Cl[C:21]([O:23][CH:24]([Cl:26])[CH3:25])=[O:22]>O1CCCC1>[OH:1][C:2]1[CH:15]=[C:14]2[C:5]([N:6]([C:21]([O:23][CH:24]([Cl:26])[CH3:25])=[O:22])[C:7]3[C:12]([S:13]2)=[CH:11][CH:10]=[CH:9][CH:8]=3)=[C:4]2[CH:16]=[CH:17][CH:18]=[CH:19][C:3]=12

参加物

4

反応物 2

HCID 5213051-Chloroethyl chloroformateHCID 137124785-hydroxy-12H-benzo[a]phenothiazine

生成物 1

HCID 146014145-hydroxy-12-(alpha-chloroethoxycarbonyl)-12H-benzo[a]phenothiazine収率 57.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 5-hydroxy-12H-benzo[a]phenothiazine (5 g) and α-chloroethyl chloroformate (10 g) in tetrahydrofuran (20 ml) was refluxed for 9 hours, then the volatile components were evaporated away and the residue chromatographed on a column of silica gel, eluting with a 1:9 ethyl acetate-hexane mixture to afford the title compound (4 g) as an oil.

後処理

  1. temperaturewas refluxed for 9 hours
  2. customthe volatile components were evaporated away
  3. customthe residue chromatographed on a column of silica gel
  4. washeluting with a 1:9 ethyl acetate-hexane mixture

出典と根拠

ORDレコード
ord-9fd6b759ef3c4c96bf939e4e003a6fb2
出典データセット
uspto-grants-1989_10
特許番号
US04876246

反応ノート

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