Trichloroacetic Acid → 2-[3-(2-chloroethyl)-2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid cyclohexylammonium salt

HRID 1651524ノート

反応式

HRID 1651524 の反応式
[Cl:1][CH2:2][CH2:3][N:4]1[CH:9](O)[CH2:8][CH2:7][O:6][P:5]1(=[O:18])[N:11]([CH2:15][CH2:16][Cl:17])[CH2:12][CH2:13][Cl:14].[CH:19]1([NH3+:25])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.[SH:26][CH2:27][CH2:28][S:29]([O-:32])(=[O:31])=[O:30].ClC(Cl)(Cl)C(O)=O>CN(C)C=O>[CH:19]1([NH3+:25])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.[Cl:1][CH2:2][CH2:3][N:4]1[CH:9]([S:26][CH2:27][CH2:28][S:29]([O-:32])(=[O:31])=[O:30])[CH2:8][CH2:7][O:6][P:5]1([N:11]([CH2:15][CH2:16][Cl:17])[CH2:12][CH2:13][Cl:14])=[O:18]

参加物

5

反応物 3

HCID 6421Trichloroacetic AcidHCID 113822203-(2-chloroethyl)-2-(bis-(2-chloroethyl)-amino)-4-hydroxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxideHCID 230498732-Sulfanylethane-1-sulfonic acid--cyclohexanamine (1/1)

生成物 1

HCID 1317149772-[3-(2-chloroethyl)-2-(bis-(2-chloroethyl)-amino)-2-oxo-tetrahydro-2H-1,3,2-oxazaphosphorin-4-yl-thio]-ethanesulphonic acid cyclohexylammonium salt

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

340 mg (1 mmol) of 3-(2-chloroethyl)-2-(bis-(2-chloroethyl)-amino)-4-hydroxy-tetrahydro-2H-1,3,2-oxazaphosphorin-2-oxide and 240 mg (1 mmol) cyclohexylammonium-2-mercaptoethanesulphonate in 2 ml of dimethylformamide were mixed with a trace of trichloroacetic acid and were stored for 2 days at -25° C. The reaction mixture was then precipitated with 20 times the quantity of ether. The residue was washed and dried.

後処理

  1. customThe reaction mixture was then precipitated with 20 times the quantity of ether
  2. washThe residue was washed
  3. customdried

出典と根拠

ORDレコード
ord-d2d27b32d42e4ba59eade8ac5293da72
出典データセット
uspto-grants-1990_05
特許番号
US04929607

反応ノート

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